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SUMMARY

This Study aims at investigating and establishing a desirable cooperation system as well as international technical information exchange measures with other countries to make the WE-NET Project a truly international cooperation project as part of the WE-NET Project which has been implemented since FY 1993 and which has been consigned by the NEDO.

As the WE-NET Project presupposes international cooperation, the major premise for the success progress of the Project is that various hydrogen energy-related organizations and people abroad properly understand the total picture and extend their cooperation for the Project. The Phase I Study identified the necessary themes for the promotion of international cooperation under the WE-NET Project by studying the trends of similar projects in related countries, the details of research work at various research institutes overseas and the hydrogen energy technology development programmes in leading industrialised countries, etc. together with activities designed to facilitate international understanding of the WE-NET Project and to promote information exchanges with overseas organizations. In Phase II, continual efforts have been made to materialise the vision of the WE-NET Project while pursuing each of the themes mentioned above.

In FY 2000, work on the following themes was conducted.

1. Promotion of International Research Cooperation

As the WE-NET Project presupposes international cooperation, it is essential that its entire idea be widely as well as accurately understood by organizations and people abroad.

In recent years, many projects other than the WE-NET Project in Japan and abroad to develop useful applications of hydrogen, particularly those for automobiles driving by fuel cells and hydrogen supply stations, etc., have begun to enter the demonstration stage. International cooperation is becoming more important than ever to ensure the speedy as well as efficient progress of demonstration work. In this context, it is essential to clarify in what way the WE-NET Project can contribute to

hydrogen-related projects overseas. For this purpose, the following activities have been conducted.

1.1 Distribution of Collection of Summaries in English of Project Achievements in FY 1999

The English version of the Collection of Summaries of Project Achievements compiled by the NEDO based on the taskforce reports for FY 1999 was distributed to 157 overseas organizations which had been listed through the regular exchange of information. In this way, diffusion of the activities under the WE-NET Project throughout the world and the establishment of a system to gather worldwide information on hydrogen was made possible.

1.2 Presentations at International Conferences

Reports on activities relating to the WE-NET Project were actively presented at the international conferences listed below to facilitate an accurate understanding of the WE-NET initiative and associated activities so that the work under the Project can walk hand in hand with similar projects in other countries.

(1) 10th General Meeting of the CHA(2) 13th Meeting of the WHEC(3) Hyforum 2000(4) Marcusevans Conference(5) 12th General Meeting of the NHA(6) Meeting of the International Hydrogen Infrastructure Committee

1.3 Research Cooperation by International Energy Agency (IEA)

The IEA is conducting basic R & D on future hydrogen technologies on the basis of a multi-lateral agreement concerning hydrogen energy. The following activities have been conducted by the IEA.

(1) Attendance at meetings of the Committee for IEA Implementation Agreement on Hydrogen Production and Utilisation

(2) Dispatch of experts to each Annex

2. International Technical Information Exchange and Other Activities

In order for the WE-NET Project to develop as an international project, the establishment of a cooperation system for the wider use of hydrogen is essential while ensuring intensive information exchange with related organizations and people abroad. The following activities were conducted in FY 2000 to expand the scope of the WE-NET Project.

2.1 Overseas Studies Relating to WE-NET Project

Each task force under the WE-NET Project conducted an overseas study in line with its objectives to gather information on hydrogen energy abroad.

2.2 Study on Development Trends of Fuel Cells

The latest situation of development of fuel cells abroad was studied, including fuel cells for automobile application which have been attracting much attention recently.

2.3 Study on Overseas Research Institutes on Hydrogen Energy

Research institutes worldwide which are engaged in R & D on hydrogen energy were studied and the details of the research work of these institutes and their access address were listed on the WE-NET Home Page. As the scope of the study in FY 1999 was not exhaustive in view of it being the first year, the study will continue to consolidate the information provided on the Home Page.

2.4 Setting Up of Japan Booth at Hyforum 2000

“Hyforum 2000”, the first major conference on hydrogen energy in Europe, was held in Munich and the Japan Booth was set up with the assistance of the MITI and the NEDO to publicise the WE-NET Project.

2.5 Renewal of WE-NET Home Page

Sections of the We-NET Home Page where the information provided had become outdated were renewed to incorporate the latest information and information on the overseas research institutes surveyed in FY 1999 and the FY 1999 WE-NET Report were added to the Home Page.

2.6 Production and Distribution of Video on Hydrogen Safety

Education on the safety of hydrogen application is essential for the realisation of a hydrogen society. The scenario for a video publicising hydrogen safety was completed in FY 1998 and the actual video was produced in FY 1999. The original English version and a voice-over version in Japanese were distributed to hydrogen- related research institutes, universities and enterprises in Japan to appeal the safety of hydrogen application.

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— 4 —

Executive Summary (Annex 12)

Introduction

The movement toward implementation of hydrogen as an alternate fuel has been an active goal among energy scientists and environmentalists since the 1973 “energy crisis”. It is for this reason that the International Energy Agency (IEA) Agreement on the Production and Utilization of Hydrogen was established in 1974. After a quarter-century, the IEA Hydrogen Agreement continues to promote this same goal. In recent years, renewed support has come in the form of increasing interest from the industrial sector, in particular oil companies and automobile manufacturers. This trend seems to have at least three sources: (1) the technical successes of several new fuel-cell companies, (2) increasing movement toward efficient and clean vehicles, and (3) a growing scientific and political realization that the long-suggested negative effects of greenhouse gases are likely real and pose very serious questions for our future. The renewed opportunity to participate in the practical implementation of “Hydrogen Energy” has been welcomed by all within the IEA Hydrogen Agreement family, but there are many technical and economic problems that remain. The IEA Hydrogen Agreement’s Task 12, Hydrogen Storage in Metal Hydrides and Carbon, was specifically targeted towards addressing the problem of “solid- state” hydrogen storage.

On-board hydrogen storage remains an undisputed problem for hydrogen-fueled vehicles. Although recent progress in metal hydride batteries has been significant, little real progress has been made in efforts to advance the room-temperature hydrogen gas storage capacity of traditional hydrides over the last 30 years. At least this statement can be made relative to the present requirements for supplying PEM fuel-cell vehicles, where high gravimetric hydrogen- storage density is required and where hydrogen must be liberated at temperatures compatible with the waste heat of the fuel-cell (<100DC). Alternatives to solid-state vehicular hydrogen storage exist, such as high-pressure gas, cryogenic liquids and onboard reforming of conventional liquid hydrocarbon fuels, but well-known disadvantages can be cited for each.

Something of a thermodynamic dilemma has evolved over the last 30 years when it comes to “conventional” metal hydride storage of hydrogen. Numerous hydrides with metallic-bonding (e g., those represented by LaNi5 and TiFe) have been developed to reversibly store hydrogen at near-ambient temperatures, but they suffer from poor gravimetric capacity (typically no more than 2 wt.% H). At the other extreme, there are ionic- and covalent-bonded hydrides (e.g., Li- and Mg-based alloys, respectively) that have good gravimetric capacities (5-10 wt.% H), but require uncomfortably high temperatures (>250DC) to release the stored hydrogen at positive pressure. There are very few known hydrides between these two extremes.

The basic hydride problem was recognized by the IEA Hydrogen Agreement Executive Committee and led to the creation of Task 12 in 1995 to seek new and different storage possibilities. Thus, the Task focused new hydride storage R&D on non-traditional hydrides. In addition, carbon hydrogen-storage media were incorporated into the Task in response to reports of new promising results. This Final Report for Task 12 thoroughly summarizes the extensive solid-state hydrogen-storage R&D work completed on behalf of IEA during the period 1995- 2000.

Duration

Task 12 was formed October 1995, with William Hoagland (USA) as the charter Operating Agent. Gary Sandrock replaced Mr. Hoagland in late 1996. Originally, Task 12 was chartered for the period Oct. 1995 - Sept. 1998, but positive results led to its extension to Sept. 2000. Originally aimed solely at metal hydride R&D, carbon was added in 1998.

Targets

The Task took aims at the following two technical targets:

1. The identification of a formulation technique for a metal hydride or carbon material that is capable of 5 wt.% hydrogen capacity with a desorption temperature of less than 100DC and a desorption pressure of at least 1 atmosphere absolute.

2. The development of a metal hydride surface treatment such that high-efficiency, reversible electrochemical reactions can be accomplished over thousands of cycles.

Target 1 centered on the potential application of metal hydrides or carbon as hydrogen-storage media for REM fuel cell vehicles, although other applications could also use such properties. Originally the temperature target was set at 150DC, but that was virtually met and superseded by a new target of 100QC during the course of the Task. Most of the Task activities were aimed toward Target 1. Target 2 concerned itself with electrochemical applications, for example electric storage batteries.

National Participations

The countries that participated in Task 12, along with the associated IEA Hydrogen Agreement Executive Committee (ExCo) members, are listed in Table I. Multiple ExCo names indicate a succession of individuals during the Task duration. Norway did not participate for the full five years of the Task. The European Commission intended to participate in the area of carbon, but its contribution was brief and never formalized.

Table IIEA H2 Annex 12 Participating Countries

and Executive Committee Members

Country ExCo MemberCanada N. BeckEuropean Commission *" A. Bahbout, G. TartagliaJapan K. Hayashi, Y. TokushitaNorway* T. RiisSweden W. Raldow, L. Vallander, K. von KronhelmSwitzerland G. SchriberUnited States N. Rossmeissl

~ never formalized* did not participate for full five years

The minimum level of effort required was 1.0 person-year/year (py/y). The actual levels of effort varied slightly from time to time, but can reasonably be represented as follows: Canada=1.0, Japan=3.0, Sweden=1.0, Norway=1.0, Switzerland=2.0, and USA=2.8.

Official Experts and Institutions

The roster of Task participants and institutions (Table II) covers a large spectrum of experience, expertise, reputation and experimental capability in the field of metal hydrides and carbon- hydrogen interactions. Those skilled in the art will recognize most of the names and institutions listed in Table II. In addition to the designated Official Experts listed in Table II, there were many other staff members, graduate students and postdoctoral scientists involved in the work. The individuals are too numerous to be mentioned here; see the List of Publications and Presentations. Note that Bogdanovic’ (Germany) and Verbetsky (Russia) participated unofficially because their countries were not formal participants in Task 12. However, they did have limited financial support from Sweden and Switzerland, respectively, as well as the IEA.

Table IIParticipating Task 12 Experts and Institutions

Canada: R. Chahine*, University of QuebecA. Zaluska*, McGill University

(European Commission*): (P. Bernier*, University of Montpellier)

Japan: E. Akiba, National Institute of Materials & Chemical ResearchS. Suda, Kogakuin UniversityI. Uehara*, Osaka National Research InstituteN. Kuriyama*, Osaka National Research Institute

Norway: A. Maeland*, Institute for Energy Technology

Sweden: D. Noreus, Stockholms University(B. Bogdanovic’, Max-Planck-lnstitute fur Kohlenforschung)

Switzerland: L. Schlapbach, University of FribourgK. Yvon, University of Geneva(V. Verbetsky, Moscow State University)

United States: M. Heben*, National Renewable Energy LaboratoryC. Jensen, University of HawaiiR. Loutfy*, MER CorporationF. Lynch*, Hydrogen Components Inc.R. Murphy*, Oak Ridge National LaboratoryG. Sandrock, SunaTech, Inc.G. Thomas, Sandia National Laboratories

* indicates not involved for full 5 years; () indicates unofficial

Projects

Task 12 consisted of a series of R&D projects aimed at particular materials and approaches toward achieving one of the Task Targets. Table III lists the 20 projects (16 hydride and 4

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carbon). Each Project had a Leader and was funded mainly by the Leader’s country. However, most of the projects involved international collaborations beyond the Leader’s home country or institution. All projects were experimental in nature except Project 7, which was a data compilation and public on-line database activity.

Table IIIList of Task 12 Projects and Leaders

No. Title LeadExpert

LeadCountry

1 Destabilized magnesium nickel hydride D. Noreus Sweden2 Vapor phase synthesized Mg2Ni G. Thomas USA3 Fine-structured RE(Mn,AI)2 alloys L. Schlapbach Switzerland4 Laves phase CaAI2_bXb alloys with substitutional and interstitial

elements XI. Uehara Japan

5 Preparation and characterization of titanium-aluminum alloys as potential catalysts for reversible alkali metal-aluminum hydrides

A. Maeland Norway

6 Structural investigations of intermediates and end products in the synthesis of Ti-doped alkali metal-aluminum hydrides

D. Noreus Sweden

7 Comprehensive hydride review and associated IEA databases G. Sandrock USA8 Mechanical destabilization of metal hydrides A. Zaluska Canada9 Ball milling under reactive atmosphere E. Akiba Japan10 Application of polyhydride catalysts to Na-AI hydrides C.Jensen USA11 High-pressure synthesis of new hydrogen storage materials K. Yvon Switzerland12 Ball milling effects during fluorination of the eutectic alloy

Mg-Mg2NiS. Suda Japan

13 Ca-based ternary alloys N. Kuriyama Japan14 Catalytically-enhanced sodium aluminum hydride C.Jensen USA15 Metal hydride safety testing F. Lynch USA16 Synthesis and structural analysis of new ternary hydrides

based on hydride-fluoride similarityE. Akiba Japan

C-1 Optimization of single-wall nanotube synthesis for H2-storage M. Heben USAC-2 Hydrogen storage in fullerene-related materials R. Loutfy USAC-3 Assessment of hydrogen storage on different carbons R. Chahine CanadaC-4 Hydrogen-carbon, hydrogen-metals L. Schlapbach Switzerland

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The projects listed in Table III are generally in order of initiation, with subdivision only as to hydride and carbon. It is useful though to group the projects into more specific categories to better explain their purposes:

Projects 5, 6, 10, 11, 14 and 15 can be collectively described as projects on complex hydrides involving mixtures of ionic species and covalently-bonded complexes of hydrogen and non­transition or transition metals. Projects 5, 6, 10, 14 and 15 involve the family of non-transition metal complexes called the alanates, principally catalyzed NaAIH4. The catalyzed alanates were brought into Task 12 as a result of the pioneering discovery of this new class of exciting materials by Prof. B. Bogdanovic’ of Germany. Project 11 has searched for new transition metal complexes using high-pressure techniques. Project 16 can perhaps also be included in this category because it resulted in the discovery of a new class of hydrides based on the Zintl phase, a kind of hybrid among ionic, complex and metallic hydrides.

Projects 1, 2, 8, 9 and 12 all look at materials based on Mg2NiH4 or Mg2NiH4-containg alloys. Mg2NiH4 can also be classified as a transition metal complex and has been known as a classic Mg-based hydride since 1968. These projects have examined some new ways to improve Mg2NiH4 properties and understanding by thermomechanical means (1), mechanical milling (8, 9, and 12) or vapor-phase synthesis (2). Although Project 12 started out to improve the hydriding and dehydriding properties of the Mg2NiH4-Mg eutectic alloy by ball milling and fluorination, it evolved into a project examining the catalytic properties of the material on the hydrolysis-driven liberation of H2 from NaBH4 complex solutions.

Projects 4 and 13 studied the relatively unexplored area of Ca-based alloys and intermetallic compounds. Project 3 discovered a new AB2 Laves-phase hydride.

Projects C-1, C-2, C-3 and C-4 widely addressed the newly active area of hydrogen in/on carbon. C-1 focused on single-wall nanotubes with an emphasis on optimizing synthesis and cutting for the purposes of hydrogen storage. C-3 and C-4 surveyed a range of available carbons relative to gaseous and electrochemical hydrogen storage, respectively. C-2 studied the potential of storing and liberating covalent-bonded hydrogen on fullerene carbons.

Communications

The keys to a successful Task are interactions, collaborations and communications among the participants. For Task 12, this was accomplished in two ways. First, every two months or so, Project Leaders provided short progress reports that were then assembled and distributed by e- mail.

The second method of communication was in the form of Experts’ Workshops that were held about twice per year, on the average. Table IV lists the official Experts’ Workshops held throughout the duration of Task 12. The first three listings represent Planning Workshops held before the formal start of the Task. Often Workshops were held in conjunction with international meetings to minimize extra travel and maximize IEA participation. The Workshops usually covered two areas: (1) necessary information transfer and (2) technical reviews of all the projects by the Leaders or their representatives. Attendance at the Workshops was excellent. In almost all cases, good direct or proxy presentations were made and all Experts were

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encouraged to interact and provide advice and comments. International collaborations were reinforced or newly established. The spirit of the IEA Workshop was fulfilled in all cases.

Table IVList of Experts’ Workshops

Dates Location21 March 1994 Washington, D C., USA12 October 1994 Miami Beach, USA17-18 July 1995 Henniker, USA27-28 September 1995 Kjeller, Norway27 August 1996 Les Diablerets, Switzerland13 March 1997 Alexandria, USA14 July 1997 Henniker, USA26 January 1998 West Palm Beach, USA

(carbon only)9-10 March 1998 Davos, Switzerland30 September - 1 October 1998 Tokyo, Japan20-21 July 1999 Henniker, USA2-3 March 2000 Davos, Switzerland6-7 October 2000 Noosa, Australia

Summary of Results Achieved

The overall result of the Task was significant measurable progress toward Target 1, as well as general progress in the understanding of metal hydrides and carbon as hydrogen-storage media. This will be only a brief summary of the principal results, project by project. Each of these projects is presented in some detail later in the form of individual Project Reports, the main summary mechanism of this Final Task Report. In addition, Publications and Presentations resulting from each Project are listed in order for interested parties to pursue even more details.

The closest approach to achieving the 100DC, 5 wt.% hydrogen-storage target resulted from the sodium alanate (hydride complex) projects. Sequential Projects 10 and 14 studied the catalyzing of NaAIH4 by mechanical (ball milling) methods using liquid and solid catalyst precursors. Preliminary determinations of engineering behavior and properties were made. By the end of the Task, 4-4.5 wt.% at 125DC was routinely demonstrated with reasonable hydriding and dehydriding rates. This is close to the target and represents a hydride capacity- temperature combination never achieved before. Related work showed the validity of the two- step NaAIH4 reaction and determined the structure of the important intermediate phase Na3AIH6 (Project 6). The exact catalyst(s) influencing the alanate reactions have not been determined, but Project 5 examined the possible structural and reaction roles of Ti3AI hydrides as catalysts. A much needed safety study of NaAIH4 was started in Project 15, but, unfortunately, was not completed. As a measure of the progress made in the IEA alanate efforts, distinct interest has resulted from outside of the IEA, including commercial interest among automotive and fuel cell companies. An example of increased national interest can be seen by the fact that Japan’s WE-

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NET project has begun the funding of independent alanate work by one of the IEA alanate Experts.

Project 16 discovered a new family of hydrides based on the Zintl-phases, e.g. SrAI2 and SrAI2H2, both of which are Zintl-phases. These new hydrides have certain similarities to the mixed ionic-covalent alanates and may offer an exciting new “nonconventional” area for future catalyzed hydride R&D.

Project 11 opened the stage for extending the catalyzed alanate work to transition metal complexes. It reported the discovery of a number of new complex hydrides. One of the most promising for future attempts at catalyzing is Mg3MnH7.

Five projects revisited the old and classic complex hydride Mg2NiH4 with aims at destabilizing it, i.e., making hydrogen desorption easier at lower temperatures. Projects 1 and 2 showed it was possible to destabilize Mg2NiH4 by lower temperature synthesis (avoiding microtwinning), mechanical working and controlling phase impurities like Mg. It also identified for the first time color and electrical resistivity changes that may have practical applications. Project 2 was performed in close conjunction with Project 1 using a newly developed method of synthesizing single-phase Mg2NiH4 by a Mg-vapor process. Projects 8 and 9 studied the effects of ballmilling. Project 8 showed that the temperature of hydrogen desorption could be synergistically lowered by ball milling mixtures of Mg2NiH4 and MgH2. Project 9 examined the ball milling of Mg2Ni in an H2 atmosphere (i.e., the formation of Mg2NiH4 while milling). Although finer products resulted, the hydride phase structure was similar to static hydriding. In summary, the four projects cited immediately above resulted in significant improvements in hydriding/dehydriding kinetics and modest increases of equilibrium plateau pressures. In general, hydrogen liberation temperatures above 200DC were still practically required, so the Task Target was not approached as nearly as the alanate work.

Project 12 was the only project in Task 12 that did not involve reversible hydriding and dehydriding. Instead it focused on the irreversible liberation of H2 by the catalyzed hydrolysis of NaBH4 solutions. It found ball milled and fluorinated Mg-Mg2Ni eutectic alloy (and its hydrides) to be promising hydrolysis catalysts.

Projects 4 and 13 searched for new Ca-based alloys and intermetallic compounds. Although several were identified, they seem to be highly prone to disproportionation and unlikely to provide much practical hope of achieving the Task Target. Similarly, Project 3 reported on the discovery of a new AB2 Laves-phase CeMnAI. It does not seem to offer practical hydrogen- storage properties, but may be useful as a hydrogen getter.

The four projects on carbon storage media provided mixed results. Projects C-3 and C-4 surveyed a number of commercially and experimentally available materials with regard to gaseous and electrochemical hydrogen storage, respectively. Although some hydrogen storage was measured, results of these two projects fell well short of confirming the high levels of hydrogen storage often noted in the literature. In distinct and credible contrast to this, Project C-1 showed promising levels of hydrogen storage in single-wall carbon nanotubes that had been properly synthesized, purified and cut by mechanical/chemical processing. Levels of around 6.5 wt.% H2 were shown, with some of that hydrogen coming off room temperature and the rest in the 200-400DC range. Next to the alanate results, this project comes closest to meeting the technical Task Target of 5 wt.% H2 at 100DC.

Project C-2 studied chemisorbed hydrogen on fullerenes, i.e., fullerene hydrides. Because of the relatively strong H=C bonding, fullerene hydrides are a thermodynamic challenge for practical hydrogen storage. However, like the catalyzed alanates, promising catalyst results were shown in the project, along with possibilities for metal atom substitution.

Finally, Project 7 (the only non-experimental project) resulted in an extensive series of on-line hydride databases (URL: http://hydpark.ca.sandia.gov). The hydride data are far more complete than any printed resource. It has become a widely used Internet resource by hydride scientists and engineers.

Future Work

The ExCo, Task 12 Experts and Operating Agent all agreed that the results of the Task 12 work were promising enough to construct a new and broader hydrogen storage task. The new proposed Task, Solid and Liquid State Hydrogen Storage Materials, has been approved and is being finalized for startup about May 2001. It will be broader in the sense that it will consider other solid and liquid storage media beyond nonconventional hydrides and carbon. It will also involve more than experimental projects, in particular theoretical, modeling and engineering activities. Additional countries, organizations and Experts will participate.

Acknowledgements

The strong support and encouragement of the ExCo members from both the participating and nonparticipating countries is greatly appreciated. Special thanks goes to participating ExCo members for their continued funding and guidance to their Experts and to the U S. Department of Energy Hydrogen Program (Mr. Neil Rossmeissl) for providing the Operating Agent. Finally, acknowledgements and thanks go to Mr. William Hoagland for his efforts in starting Task 12.

Activities ReportPrepared for the May 2001 Executive Committee Meeting

Preparation Date: April 6, 2001

IEA Hydrogen Implementing Agreement’s Annex 13 DESIGN AND OPTIMIZATION OF INTEGRATED SYSTEMS

The objective of Annex XIII is to provide a means to increase energy independence, improve domestic economies, and reduce greenhouse gas and other harmful emissions from stationary and mobile sources. Emphasis will be placed on comparison of systems with respect to efficiency, environmental impact, capital and operating costs, and other measures of importance.

Activities during the Previous Six Months

ANNEX 13 EXPERTS MEETING, ISPRA, ITALY (APRIL 3-4, 2001)

The fifth meeting of the Annex 13 experts was held in Ispra at the Joint Research Council (JRC) facilities. Participants in attendance included Canada, the EC, the Netherlands, Norway, Spain, Sweden, and the USA. We were pleased to have Switzerland as an observer/participant to our meeting. As was the case for the fourth meeting last Fall, neither Japan nor Lithuania was able to attend.

Annex Work Plan Review - Status of ActivitiesActivity A1: Component Model Development and Improvement (Activity Leader - USA)The status of model improvement was discussed and revision needs were compiled. In the production area, there is a need for a model of the autothermal process (Transportation Systems). We would also like to include a more detailed handling of the bipolar (pressurized) electrolyser case (Remote Systems) and efficiency curves for partial load for various electrolysers (GHW can operate at 20-100%; Norsk Hydro can operate at 50-100% power; and Stuart Energy can operate at 20-120%). The accuracy of small-scale reformer costs (Transportation Systems) that are available in the literature was brought into question, given what appears to be the use of a common (single) scaling factor for large and small-scale systems (not appropriate due to the difference in heat integration and overall system efficiency). Developers of small-scale reformers (Idatech, Praxair, IFC, Gastech-Plug Power) will be contacted to try to get additional input into cost and efficiency information.

In the storage area, we need to address the non-steady-state aspects of storage. Compressors associated with compressed hydrogen storage/delivery systems need to be modeled in such a way as to determine the best operating procedure (Transportation Systems). The state-of-the-art in liquid storage needs to be incorporated in our liquid storage models to better determine the rates of boil-off.

The transfer of hydrogen from delivery systems to stationary storage and/or to the end-user also results in some losses. The negative perceptions from the use of robotic refueling for liquids hydrogen (BMW experience) was discussed. Although it is technically feasible to develop a robotic refueling device, this imparts a perception that liquid hydrogen refueling is unsafe. Harmonized regulations as developed in the El HP Phase 1 and other efforts were also identified as an important activity to which we must pay some attention.

Finally, there was discussion of the distribution of hydrogen in pipeline systems, including the extent to which hydrogen can be added to natural gas (10% had no effect except for some end

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use applications). There is also interest in long-distance hydrogen pipelines (the Asia Pipeline Project).

Activity A2: Cost Model Development (Activity Leader - Canada)Five spreadsheets have been developed: Component Model Description; Local Conditions (one for each of the case studies); Initial Investment Costs; Annual Costs; Cost Model (this is linked to the other spreadsheets). The discussion centered on several issues regarding definitions and needs. The working capital was defined as the amount of money required to “balance the books” at the end of Year 1. This is the amount of money that keeps the project “in the black,” and is important for investors and bankers, as well as policy makers. An alternative definition used in some analyses (in the US) is approximately one month’s payables (invoices and labor). Clarification is required to insure that uses understand what is meant by working capital in our studies.

Data are required from each of the case studies regarding the component costs. The level of detail in costing may vary for the components. Team Leaders are to take charge of collecting and formatting the costing information, and for forwarding the cost models to Canada as they are generated.

Activity B1: Design and Optimization of Hydrogen Systems (Activity Leader - The Netherlands) The objectives of the activity were reviewed and discussed for each of the case studies. The three objectives are: identification of design issues; identification of technologies that require improvement; and identification of interesting aspects for demonstration. The objectives in relation to the three case studies (Residential Systems; Remote Communities, and Transportation Systems) are summarized in Table 1 following the discussion each case study (see below).

Residential SystemsThe Team Leader for this system is The Netherlands. Frans Tillemans presented the results of a number of configurations for a greenfield residential community.

The development of greenfield communities is an important opportunity for hydrogen energy systems. In the Netherlands, new residential districts are being developed, with housing additions of 60,000 (1-2% of the total housing market of 6 million). There is an ambitious national plan to require the power generation mix to include 3% renewables (green energy) by 2010 and 10% renewables by 2020. The Dutch national energy policy includes price supports via an eco-tax of up to 30% on non-green energy. Given the requirement to integrate renewables in the national power mix, continued deregulation of utilities, and the desires by many communities to include “green” homes, hydrogen systems offer interesting opportunities for residential developments.

Introducing hydrogen as an energy carrier requires a different infrastructure from the existing infrastructure. Developing such an infrastructure for mobile applications is a much-debated issue. For stationary applications, the role of hydrogen is less defined but will likely depend strongly on the introduction strategies for fuel cells. The first large-scale application of fuel cells may well be small-scale combined heat and power (CHP) systems. One interesting starting point for developing a hydrogen infrastructure is the use of hydrogen as a fuel for CHP units based on fuel cells. To fully realize the ultimate clean-energy benefits, hydrogen energy systems will use hydrogen from renewable sources. However, in the nearer term, H2 will most likely be produced from fossil fuels. The availability of appropriate technologies to support a

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hydrogen energy system based on fossil fuels is one important aspect of this early-introduction strategy.

Remote CommunitiesThe Team Leaders for this system is Norway. Ronny Glockner presented the results of a wind- hydrogen system with three designs.

Hydrogen energy systems have been proposed as a means to increase energy independence, improve domestic economies, and reduce greenhouse gas and other harmful emissions from stationary and mobile sources. These systems, however, face technical and economic barriers that must be overcome before hydrogen can become a competitive energy carrier for the 21st century. A wind-H2 system for a remote location was studied to determine the feasibility of producing hydrogen for transportation applications. This case study was initiated by STATKRAFT SF, Norway’s largest producer of hydroelectric power and the second largest producer in the Nordic region. The modelling work was performed by the Institute for Energy Technology (IFE).

In Norway, more than 99% of the electricity demand is supplied by hydropower. During the last 10 years, however, public resistance based on environmental issues has virtually brought the development of the remainder of these resources to a standstill. Because of the increase in power demand and good wind resources along a sparsely populated coastline (a potential of around 10 TWh/year is recognised), the focus on wind energy plants has grown over the last years. It seems that the public resistance, especially in the early phase of the introduction of large-scale wind energy development, is smaller than is the case for further hydropower development. Over the last year (2000), the Norwegian government has approved several applications for building of wind parks, in total amounting to some 300 MW peak power.

The selected locations for Norwegian wind parks are remote areas, such as islands, where the best wind resources are found. The wind parks will produce power for the small communities in these areas, but also for the common electricity grid as a complement to the existing hydropower. In this study, the production and use of hydrogen in fuel cells in relation to such wind parks is discussed. A wind/electrolyser-based hydrogen refuelling station taking the base power from one of the large windmills in a wind park is modelled. The hydrogen produced is assumed to be used in buses operating the public transport on the remote location. At a later stage, hydrogen for operation of ferries would also be an attractive alternative.

Transportation SystemThe Team Leader for this system is USA. Susan Schoenung presented her analysis of a number of refueling configurations for hydrogen vehicles.

The goal of the Transportation Systems case study is to address specific hydrogen demonstration opportunities with respect to energy independence, improved domestic economies, and reduced emissions. The transportation analysis is not as geographically specific as the other two case studies. The overall scope of the analysis includes comparison of hydrogen passenger vehicle fueling options including refueling alternatives (primarily various sources of liquid and gaseous hydrogen), vehicle configuration alternatives (primarily various hydrogen storage and power plant configurations), drive cycle implications, and cost variations ( electricity, natural gas, and hydrogen).

Figures of merit for the project are costs (capital and operating), efficiency (vehicle fuel economy and overall energy efficiency), footprint, and emissions.

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Table 1: Review of ObjectivesCase Study Design Issues Technology Improvements Demonstrations

Residential Peak heat is difficult to supply with a PEMFC• 80C heat available for

65C requirement• Seasonal not diurnal

Heat pumps need to be cheaperSmall reformers would allow combined fuel and heat production

Integration of heat and electricityLossesPublic perception

Remote Minimize cost and emissions for stand alone system by using larger wind farms or hybrid systemsLoad-following electrolysers Wind-diesel or -NG hybrids Hydrogen as a fuel for generator setsLoad-leveling for weak grids

Metal hydride storageCost scaling for electrolysis Compressor

Wind-electrolyser connection (check RAL project)

Transportation Capacity factorsParametrics“Safe Distance” and C&S requirements

Autothermal reformersPOX reformers (not enough detail to make model)

Refueling stations

Clarification of Objectives

Optimization criteria• Efficiency• Emissions• Cost

Research areas Policy concerns VerificationMotivation

Activity B2: Life Cycle Assessments (Activity Leader - Japan)The Team Leader was not present at the Experts Meeting. The USA, Switzerland, and the EC presented recent LCA work.

The Wind-Electrolysis life cycle assessment (LCA) carried out in the U.S. was presented as a basis upon which the detailed LCA of the Remote Systems cases could be evaluated. An LCA, performed by the EC, for the production and delivery of liquid hydrogen to a cryoplane stationed in Sweden was also presented. Some very interesting presentation techniques were used, and will likely be used for all reports. The interpretation of results, and communicating these results to our clients, is essential. The vehicle LCA, presented by Switzerland, is the product of the doctoral thesis of Alexander Boeder. The presentation materials are to be kept confidential until the report is released by PSI in May 2001. The results are very useful to our efforts, and provide an important contribution to our efforts.

The EC will lead the LCA effort for the Transportation Systems case study, incorporating the Swiss contribution. The USA will lead the LCA for the Remote Systems case study, with clear identification of the systems of primary interest from the Team Leader, Norway. Both the EC and the USA will work together to perform the necessary LCA studies for the Residential Systems (a reduced number of cases will be selected with the help of the Team Leader, The Netherlands. There is some interest to include a biomass case in the LCA, since a great deal of effort in this area has been performed regarding LCA.

Demonstration Project ReportsThomas Schucan, under the direction of the IEA Hydrogen IA Secretariat, is developing a second edition of the highly successful hydrogen demonstration reports (Subtask A from Annex

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11). The current list of new projects was presented and the status of each report was discussed. Currently, contact has been made, and agreement to participate received, from the following projects:- SunLine (USA) Transit Bus Demonstration

Hamburg (Germany) Hydrogen Fuel Cell System- Grimstad (Norway) Renewable Hydrogen System

Bavarian (Germany) Fuel Cell Bus- Georgia (USA) Bio-oil Reforming Project- W.E.l.T. (Germany) Hydrogen Delivery Vans

Several other projects were identified as likely, or extremely desirable, participants:- Vancouver (Canada) Bus Project

Ford (USA) Refueling Station- World Bank Bus Projects in Mexico, China, India, Brazil, and South Africa

California (USA) Fuel Cell Partnership Activities- Spanish Project (presented at NHA meeting)- Japanese Refueling Stations

information was also provided on European hydrogen projects in Germany and Sweden, including the development of a methanol fuel cell for a mobile phone.

Major Accomplishments

Two manuscripts, one on the Remote Systems case study and one on the Residential Systems case study, were completed and submitted for publication in the proceedings of the World Energy Congress to be held in Argentina in October 2001. Presentation of the Transportation Systems case study have been made and additional presentations are planned, including at the Canadian Hydrogen Association meeting in June 2001. A number of technical papers and reports based on Annex 13 efforts have been written by the experts.

Status of Milestones

Excellent progress has been made and all milestones are expected to be completed on time.

Plans for the Next Six Months

Norway has offered to host the next Experts Meeting near Oslo, Norway. The proposed dates are October 15-16, 2001. It is anticipated that a visit to the demonstration site may be possible at that time. This is the last meeting of Annex 13 according to the original Work Programme.

It is likely this meeting will be held right before the Fall Executive Committee Meeting. The Experts are significantly limited in their collective ability to find any other dates that can accommodate all of the Experts. Normal reporting requirements for the Executive Committee will be met to the best of our abilities.

Interactions with Other IEA Groups

Annex 13 Experts participate iri other IEA Implementing Agreements, and these activities contribute in a positive way to the success of Annex 13. In particular, we are active in the Advance Fuel Cell Implementing Agreement, in particular in the Stationary Fuel Cell Annex. We have also been asked to provide input and comments on the Work Programme for Fuel Cell Systems for Transportation (AFC IA Annex XV). We have also provided information on the economics of biomass-derived hydrogen to the Bioenergy Implementing Agreement’s Gasification Annex.

Effectiveness of Task Participation

Task participation has been excellent for most of the participants. Experts are well-prepared for the meetings, and significant work effort is accomplished at the meetings. In between meetings, work continues at an excellent pace, and exchange of information and response to requests are timely. The absence from the last 2 meetings (Japan) and last 4 meetings (Lithuania) is a concern.

Matters Requiring Executive Committee Attention

Participation in Experts Meetings by all participants must be encouraged. The contributions of Experts from Japan and Lithuania are important to the success of the Annex.

Extension of Annex 13 beyond December 2001Given the recent addition of Sweden, the renewed interest of the EC in our activities, and the inquiries from Mexico and New Zealand regarding participation, it was suggested that the Annex should be extended for an additional period of at least 6 months, or perhaps one year. Some concern was expressed from several of the experts that continued participation beyond the current 3-year cycle would be difficult for their countries. An extension of 6 months would allow us to hold our final meeting at the World Hydrogen Energy Conference in Montreal, Canada (June 2002). We would also expect to present our results at this meeting.

Possible New ActivitiesThe experts proposed a number of potential new activities to be considered.

Seminar SeriesA new activity consisting of a series of seminars and plant visits was proposed. This would mirror the seminar series of Annex 11 that were found to be extremely helpful to the Experts and to those who presented seminars and/or technical tours. Concern was expressed that an informal work effort such as this could be a problem for some of the participants. Other participants noted that garnering support for this forum might be easier for them, as this would be viewed as an excellent networking opportunity. The Solid Oxide Fuel Cell Annex in the Advanced Fuel Cell Implementing Agreement has a similar structure. Details of the SOFC work plan will be provided by Sweden. The product of this new effort would be additional reports on hydrogen demonstrations.

Ideas for New Annexes- Development of curriculum for university-level process design class using models and tools- Targeted application of results of Annexes 11 and 13 (industry-led case studies)- Hydrogen demonstration project validations using modeling tools- Risk assessment/stochastic modeling/incorporating uncertainty

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- Safety and socioecomonic consequences of energy use- Public acceptance of hydrogen systems- Future trends including manufacturability and technology improvements

The Experts were approximately evenly split as to the preferred mechanism.

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Activity ReportIEA-H2 Annex-14

Photoelectrolytic Production of Hydrogen

Prepared for: Executive Committee Meeting of IEA-H2, Den Haag 9-11 May 2001Prepared by: Andreas Luzzi, Operating Agent Annex-14 (girasola@cyberone.com.au)

Introduction

This report summarises the Annex-14 activities of the period from November 2000 to April 2001, during which a number of material advances have been made. The objective of the three-year R&D program of Annex-14 is to significantly advance the fundamental and applied science in the area of solar-driven photo-electrolysis of water.

Activities

The main activities during the half-year period included:• To organise and conduct the 2nd Annex-14 expert meeting (1-3 November 2000).

• To expand the group of Annex-14 collaborators by inviting non-member countries.• To solicit and prepare Annex-14 subtask specialty summary reports.Further activities included:• To assist the IEA-H2 secretary in the expansion of IEA-H2 membership.• To assemble status-quo knowledge regarding pipeline-base transport of hydrogen.

Subtasks Progress

The key progress concerns material science and systems advancements, both contributing toward the compilation of various subtask specialty summary reports.

Subtask A

The development of effective and, above all, stable photocatalysts for water oxidation and photooxidation of organics (detoxification) progressed well. Work has been focusing on the development of thin films using nanocrystalline titania (Ti02), nanostructured polycrystalline tungsten trioxide (W03), iron oxide (above all hematite Fe203), and, as a new stream of effort, a broad range of mixed-oxides (for example iron, titanium, cerium and molybdenum).At the Swiss Federal University of Technology (EPFL), where the development of Ti02- based two-photon solar devices continues, progress has been made in the two areas of performance-improved, ruthenium-based dyes and of Fe203 as an encouraging alternative photoanode to W03.Novel Ru-based sensitisers containing functionalised hybrid tetradentate ligands were synthesized and characterized at the EPFL for Ti02 mesoporous electrodes. Most notably, these new "black" sensitizers are stable and display a significantly enhanced

Annex-14 Activity Report by A. Luzzi (April 2001)

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spectral response in the entire visible and near-IR region of the sunlight spectrum and therefore have the potential to lead to increased overall efficiency of dye-sensitized solar cells.The EPFL researchers managed to produce stable photocatalytic Fe203 layers deposited on conducting glass using a spray pyrolysis method. The Ti-doped Fe203 films produce a photocurrent of over 2 mA/cm2 under simulated AM-1.5 sunlight using water as electron source. Once coupled to an appropriate tandem photo-electrochemical (PEC) solar cell system, this result corresponds to a solar-to-chemical conversion efficiency of about 3%.Improvements in the morphology and selective doping of the Fe203 thin-films are needed to achieve higher photocurrents (short-term aim: 3 mA/cm2). Experts from the University of Uppsala (UoU; Sweden) and the University of Augsburg (UoA; Germany) have been developing highly-structured nanofibre films that promise such performance improvement. In addition, researchers at the National Institute of Materials and Chemical Research (NIMC; Japan) and the Academy of Material Science (UNAM; Mexico) are studying the effects of doping of various semiconductor thin-films. This will lead to insight into how to "tune" the conduction and valence bands of the semiconductor materials of interest to PEC devices.At the University of Geneva (UoG), a new production process for multi-layer W03 thin films with an overall thickness of typically about 3 nanometers has been matured and patented. The W03 thin films are highly transparent (60% - 80%) and consist of a network of preferentially oriented nanocrystals. They demonstrate the ability of this semiconductor to operate as both efficient and stable solar-driven photoanode for oxidation of water (so far with an efficiency of about 2.7%) and various organic compounds (eg. methanol with close to 5% efficiency). The resistancy against photocorrosion in aqueous solutions has been confirmed over a large range of pH, including strongly acidic solutions.Advanced dye-sensitised zeolite-L sandwiches have been synthesised at the University of Bern (UoB; Switzerland). These nanocrystal-sized cylindrical structures act as artificial antenna systems for light harvesting as well as transport. Using a three-dye antenna, light harvesting over the whole visible spectrum with subsequent energy transport leading to fluorescence at the zeolite-L ends has for the first time been demonstrated. Attempts are being made to use this system for the development of a novel thin-layer solar cell in which light absorption and the creation of an electron-hole pair are spatially separated.

Subtask B

The concept of combining multi-junction semiconductor devices with an electrocatalyst into a single monolithic device is being studied at the National Renewable Energy Laboratories (NREL; USA), the University of Hawaii at Manoa (UoH; USA) and UNAM.As a starting point, NREL researchers identified gallium indium phosphide (GalnP2) as a prime semiconductor for a PEC device in conjunction with gallium arsenide (GaAs). Substitute routes for GaAs are however being investigated (eg. pH change and metal-ion- treated p-type GalnP2). At the UNAM, amorphous silicon / amorphous silicon carbide (a- Si / a-SiC) shows promise for stable thin-film PEC systems. While GalnP2 / GaAs systems proved to split water with very high efficiencies (-16%), the a-Si / a-SiC system has been proven to protect a-Si-based multi-junction systems from surface oxidation, hence enhancing the viability of using this potentially cost-effective PEC cell architecture. PEC efficiencies of about 7% have been confirmed in laboratory-scale test cells.Iridium (Ir) when deposited as a co-catalyst on Ti02 was newly established as thus far best performing inorganic oxidative water-splitting photocatalyst for the dual-bed PEC reactor concept under development at the Florida Solar Energy Centre (FSEC). Work has progressed to build an electrochemical equivalent of a perforated tandem dual-bed system that uses perforated printed circuit boards and an interdigitated array of Nickel (Ni) wire.

Annex-14 Activity Report by A. Luzzi (April 2001) Page 2 of 4

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Annex-14 Experts Meeting

The 2nd Annex-14 expert meeting was conducted at the Swiss Federal University ofTechnology in Lausanne (EPFL) during the end of last year (1st - 3rd of November 2000).Hosted by the EPFL, seventeen experts from seven countries (China, France, Japan,Mexico, Sweden, Switzerland and the USA) participated in this meeting.Some of the key results and resolutions of this meeting are as follows:• Fe203 shall become the materials focus as photocatalyst for water oxidation as it is

seen as most promising regarding performance and cost. Increased collaboration is planned between EPFL, UoU, UoA, UNAM and NIMC.

• The (Revolution performance of zeolite-L silver clusters (UoB) shall be compared on a one-to-one basis with W03 and Fe203.

• Photoactive cathodes based on Ti02 (EPFL tandem system) and organic pigments (FSEC dual-bed system) are maintained as viable options for total system design.

• Monolithic semiconductor / electrocatalyst tandem systems in general remain seen as most-realistic near-term option for a first "high-performance" demonstration system. The dye-sensitised Ti02 tandem cell however appears to have better potential for cost-reduction in the long-run. Materials and systems collaboration will be intensified among UoH, NREL and UNAM for the monolithic system and UoB, EPFL, UoG, UoU and UoA for the dye-sensitised system.

• The 3rd expert meeting might be organised either in conjunction with the 10th International Conference on Unconventional Photoactive Systems (UPS'01), scheduled for the period of 4 - 8th September 2001 in Les Diablerets, Switzerland, or else in conjunction with the 7th International Conference on Advanced Materials, scheduled for the period of 26 - 30th August 2001 in Cancun, Mexico.

Membership Drive

As a result of the 2nd Annex-14 expert meeting, five groups expressed interest in either joining the H2 Implementing Agreement and/or Annex-14 in general, or else in collaborating with specific groups of Annex-14.China Being already strongly collaborating with EPFL, Day Songyuan of the Chinese Academy of Science expressed interest in joining Annex-14.France According to Claude Levy-Clement, the National Centre for Scientific Research (CNRS) has started work in electrophotochemistry some three decades ago, but then choose to shift away toward photovoltaics. Supported however by the broad experience of her team in thin-film electrochemistry, Claude is interested to collaborate with Annex- 14.Germany As a strong research team in the development and characterisation of metal oxide thin-films, the team around Armin Reller and Anke Weidenkaff from the University of Augsburg (UoA) are already collaborating with the three Annex-14 teams from Switzerland. A membership in Annex-14 seems hard to establish due to Germany's reluctance to join the IEA-H21 A.New Zealand Meridian Energy and Industrial Research Ltd. have teamed-up to apply for active membership of the IEA-H21 A. Research interest focus on Annex-13 type projects.Norway Though due to a last minute commitments he could not participate in the expert meeting, Georg Hagen from the Norwegian University of Science & Technology (NTNU) in Trondheim maintains his interest to join the Annex-14 actively.

Annex-14 Activity Report by A. Luzzi (April 2001)

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SolarPACES Task-ll

The 15th Annual SolarPACES Task-ll (SolarChemistry) workshop is planned for the 21st of June 2001 in Cologne, Germany. It is planned to present Annex-14 work on photolysis of organic pollutants in water and to discuss collaboration options.

H2 Transportation Forum

The 1st Hydrogen Transportation Forum has been scheduled for the period of 27th - 28th of November 2001 in Tokyo. It aims to assemble to assemble and assess the technology status quo and barriers to large-scale transportation of hydrogen.The OA of Annex-14 has been in contact with various interested groups around the world to assemble a preliminary spectrum of information on this topic. The key projects of the past include the Euro-Quebec Hydro-Hydrogen Pilot Project, the Huls Hydrogen Pipeline Network, the Solar Hydrogen and Electrical Energy Trans European Entreprise and the WE-NET program, with the most recent addition being the BMW Group's Solar Hydrogen Project in Dubai (project partners include Linde, Mannesmann, Siemens and E.ON Energie AG).

Collaboration Within Annex-14

Collaboration within Annex-14 member groups has generally been well, notably between EPFL - UoG, NREL - UoB, UoU - FSEC and NREL - UNAM. The exchange of ideas and materials was intensified as a result of the 2nd expert meeting in Lausanne.

Issues Requiring ExCo Attention

The Annex-14 Operating Agent asks the ExCo to consider the following issues:• Outstanding signature of the National Participation Letter of the USA.• Discussion of photoelectrochemical demonstration system options (Annex extension),

expectations and associated financial support by ExCo and governments.• Decision on participation (IEA-H2 scope and delegation) in the Hydrogen

Transportation Forum.

Annex-14 Activity Report by A. Luzzi (April 2001) Page 4 of 4

Activity Report IEA Hydrogen Agreement

Prepared for the May 2001 Executive Committee Meeting

Preparation Date: April 26, 2001By

Peter Lindblad (OA; Uppsala, Sweden)

Annex 15

PHOTOBIOLOGICAL HYDROGEN PRODUCTION

Annex 15 was approved in May, 1999 with initially four committed, participating countries: Japan, Norway, Sweden & USA. Since then Canada has joined the Annex.

The Task carries out collaborative research activities on "biophotolysis", i.e. the biological production of hydrogen from water and sunlight using microalga photosynthesis. The overall objective is to sufficiently advance the basic and early- stage applied science in this area of research over the next five (3 + 2) years to allow an evaluation of the potential of such a technology to be developed as a practical renewable energy source for the 21st Century.

The work in Annex 15 is divided into four Subtasks;

A. Light-driven Hydrogen Production by Microalgae. Activity Leader: Sweden.

B. Maximizing Photosynthetic Efficiencies. Activity Leader: USA.

C. Hydrogen Fermentations. Activity Leader: Japan.

D. Improve Photobioreactor Systems for Hydrogen Production. Activity Leader: USA.

1. Activities during the Previous Six Months

1.1. A successful ExpertsMeeting was held March 26-27, 2001 in Porto, Portugal with 8 active participants (see below). The agenda of the Expertsmeeting is enclosed as Appendix 1.

Participants March 26-27 (2001) were:

Hallenbeck, Patrick; Univ Montreal, Canada Janssen Marcel; Wageningen Univ The Netherlands Kallqvist, Torsten; Kjelsas, Norway Lindblad, Peter; Uppsala Univ, Sweden Seibert, Micheal; NREL, Golden, USA

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Tamagnini, Paula; Porto, Portugal Van Ooteghem, Suellen; NETL, USA Wright, Philip; Edinburgh, UK

Unfortunately, no representative of Japan participated in the meeting. However, we did receive (during the meeting) a fax (from Asada) presenting on-going Biohydrogen activities in Japan (see below). Komel Kovacs (Hungary) and Paula Pedroni (Italy) were unable to participate.

1.1.1 Highlights from the presentations

A) Present Biohydrogen activities in Japan.

For the last 2 years, Prof. Igarashi (University of Tokyo) has been conducting BREEZE (combination of biological hydrogen production and utilization) with financial support of Japan Bioindustry Association, which is under control of Ministry of International Trade and Industry. Although it is not easy to form a larger BioHydrogen fruit from a seed of BREEZE, Prof. Igarshi's group is going to apply to Green Chemistry as a part of the big project that will be promoted by MITI. This fact suggests that we may have some hope for a national project of BioHydrogen again.

The following is the content of the BREEZE report of this fiscal year 2000:

Chapter 1: Hydrogen production by degradation of organic wastes1-1 by pure culture (Nishio, Hiroshima).1- 2 by mixed culture (Igarashi & Ueno, Tokyo)

Chapter 2: Useful product from C02 by using hydrogen-utilizing bacteria2- 1 Analysis of C02-fixation in hydrogen-utilizing bacteria and production of

useful materials (Ishii & Aoshima, Tokyo)2-2 Ethylene production from organicwastes and C02 (Ogawa, Kumamoto)2-3 C02-utilization byusing decarboxylastingenzymes (Nagasawa, Gifu)2- 4 Useful materials from hydrogen and C02by using newly-isolated bacteria

(Morikawa, Osaka)

Chapter 3: Analysis of structure and function of hydrogenase and its application3- 1 Structure and function of hydrogenases (Higuchi, Kyoto)3-2 Probability of stabilization of hydrogenase (Nishihara, Ibaraki)3- 3 Probable application of hydrogenases (Kimura, Toyota)

Chapter 4: Construction of "Energy Metabolic Engineering"4- 1 Concept of "Energy Metabolic Engineering" (Hattori & Ueno, Tokyo Gas

& Tokyo U)4-2 Analysis of hydrogen energy metabolism with genome informatics and

construction of utility cassette (Ishii, Tokyo)4-3 Use of electric power for biological reaction (Saiki, Central Res. Inst.

Electric Power Industries)4-4 Probable application of sulfur compounds for biological energy source

(Shigeno & Murakami, Idemitsu Petroleum)

— 9.F1 —

4-5 Chemical industries and C02 & energy problems (Kawada, Daicel Chemical)

4-6 Environmental assesment of current biological technologies (Honya, Ishikawajima Heavy Industries)

4-7 Technolgy assesment of Energy Metabolic Engineering (Hattori, Tokyo Gas).

In addition, Dr. Jun Miyake's group is working on a hydrogenase from Dr. Zorin (Russia) for hydrogen production.

B) Present Biohydrogen activities in Canada (Patrick Hallenbeck).

In Canada, a team is being organized to develop, using manipulation of microbial physiology, genetic engineering and advanced bioprocess engineering, an optimal system for the biological production of hydrogen through fermentation.

Hydrogen production by fermentation. Fermentative processes, using eitherbiomass obtained in a first stage light conversion process or perhaps more attractively, various waste streams, present an interesting yet largely unexplored avenue for the biological production of hydrogen. Much is presently known about the molecular biology and biochemistry of the hydrogen producing enzymes, reductant generating systems, and physiology of many hydrogen producing organisms. The enormous

potential of metabolic engineering for redirecting electron flux to hydrogen production in various microorganisms remains to be exploited. Very little is presently known about the currently attainable yields or the possibilities for improving these yields in the future. These questions will be addressed in currently proposed research activities.

The program will be multi-disciplinary involving researchers with expertise in recombinant DNA technology, biochemistry and microbiology, and chemical and bioprocess engineering. The research program, in which various avenues will be used to generate strains capable of high levels of hydrogen production, will involve several distinct phases over five years. Finally, near the end of the initial granting period, a conceptual system in which biohydrogen production is integrated with energy production (Fuel Cell) systems will be subjected to an energy balance analysis. One line of investigation, to be carried out in the laboratory of Dr. P C. Hallenbeck will be to examine the role of microbial metabolism in limiting hydrogen production, and determining ways to overcome natural metabolic gating to the hydrogenase enzymes. In the laboratory of Dr. D. Levin, entire operons encoding ^-producing pathway gene products will be cloned into microorganisms that are optimized for large-scale bio-fermentation. In Dr. Daugulis’ laboratory the macroscopic factors that directly affect productivity, namely the cell concentration and the specific rate of product formation, and their interaction(s) in the strains

ORGANISMS)

under investigation will be examined in order to maximize the volumetric productivity of the biohydrogen process.

C) Present Biohydrogen activities in The Netherlands (Marcel Janssen)

The Netherlands are involved in two projects on biological hydrogen production. The first project is the EU ‘Biohydrogen’ project aiming at the production of hydrogen from energy crops and wastes employing (hyper)thermophilic and photoheterotrophic microorganisms. Theoretically a production of 12 moles of hydrogen per mole consumed glucose can be reached. The raw materials utilised for the production of fermentation feedstock are derived from an energy crop yielding mostly sugars and lignocellulose or waste streams yielding mainly cellulose.

The Dutch agrotechnological research insitute ATO started assessing the technological adaptations needed to enable the smooth operation of a fermentation running on the feedstock. At the same time, continuous (hyper)thermophilic fermentations are done on a smaller scale for the selection of the best performing organisms. Also Wageningen University (WU) is working on the same thermophilic fermentation employing specialist microorganisms or isolating new strains of hydrogen-producing microorganisms. The research concerns optimisation of growth and production methodologies. In addition, research is conducted on the photoheterotrophic fermentation. The efficiency of this second- stage fermentation already reached 60% with respect to the conversion of biomass (acetic acid) to hydrogen. Furthermore, 2.7% of the light energy absorbed is stored as hydrogen gas.

In the Netherlands a second project started in November 2000 on biological hydrogen production. This is a so-called EET-project and it is focused on the same production process as described above. In this project 10 Dutch partners are involved and the work is commencing as planned.

Besides these two running projects, other groups in the Netherlands are also working on biohydrogen related subjects. That is the reason why one year ago a Dutch network on biological hydrogen production was started with representatives from several research institutes (Table 1). This network is working very well. In the next months a study will be done on the state-of-the-art and perspectives of biological systems for the production of renewable hydrogen and methane in the Netherlands. In april 2001 already the 5th meeting will take place at the Catholic University of Nijmegen (KUN).

Table 1: Members of the NL contact group on biological hydrogen production

Member: R & D Institute: R&D fields:Dr. S. Albracht E C. Slater

Institute/Biochemistry, University of Amsterdam

Hydrogenase; characterisation of active site & reaction mechanism

Dr. A.J.M. Stams and Dr.E. van Niel

Laboratory ofMicrobiology,Wageningen University

FL-production extreme thermophiles and microbial CO conversion to Ha

— 9.7 —

Dr. R.H. Wijffels and M. Janssen, MSc.

Food and Bioprocess Engineering Group, Wageningen University

Photoheterotrophic H2- production and photobioreactor developmen

Dr. P. Claassen Dept, of Bioconversion, AgrotechnologicalResearch Institute (ATO)

H2-fermentations

Dr. F. Hagen Kluyverlaboratory for Biotechnology, Delft University of Technology

Enzymology

Dr. J. Keltjens Dept, of Microbiology, University of Nijmegen (KUN)

H2-fermentations; physiology and regulation H2-metabolism

Dr. T.A. Hansen Groningen Biomolecular Sciences andBiotechnology Institute

Physiology anoxygenic phototrophs

Ir. A. de Groot, J.H. Reith, MSc. And E. van Zessen, MSc.

Netherlands EnergyResearch Foundation (ECN)

evaluation H2-production systems and photobioreactor development

Dr. A. Kipperman Dept, of New Energy Technologies, NL Agency for energy and the environment (NOVEM)

promotion & support renewable energy R&D

D) Present Biohydrogen activities in USA (Mike Seibert & Snellen Van Ooteghem)

From the USA, two different approaches were presented and discusses:

(a) Two stage system using green algae (Chlamydomonas). The overview of the system concentrated on sulfur deprevation, oxygen sensitity, sequencing of the structural gene encoding the hydrogenase, and genetic approaches to delete antenna complexes. The overall project/system was recently presented in a nice review, enclosed as Appendix 2.

(b) Biohydrogen activities at National Energy Technology Laboratory (NETL)

NETL is the newest of a complex of Department of Energy Laboratories within the United States. This organization sponsors a number of technologies designed to further the goal of developing a viable hydrogen economy. NETL is also the home of the Bio-Environmental Laboratory, where work is ongoing to produce hydrogen biologically using thermophiles of the order Thermotogales.

The most recent experiments indicate that in batch experiments, Thermotoga neapolitana is capable of producing hydrogen from glucose with 71+ 24% efficiency in the presence of oxygen. This greatly exceeds the limit of 20% efficiency anticipated from fermentations. The yield of hydrogen is much lower with T. neapolitana when the organism is treated as an obligate anaerobe (as it is considered to be in the literature).

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Future work will focus on further determining exactly what metabolic pathways T. neapolitana use to catabolize substrates, and the optimal conditions necessary to obtain maximum hydrogen yield from a continuous culture of this organism.

E) Present Biohydrogen activities in UK (Phillip Wright)

The Biohydrogen activities at Heriot-Watt Universit (Scotland) are concentrating on combining molecular studies and larger bioreactor experiments. Lyngbya majuscula, is a tropical marine filamentous non-heterocystous marine cyanobacterium which is responsible for the formation of toxic algal blooms, produces over 150 novel natural products (37.5% of all natural products from marine cyanobacteria) and has the ability to fix nitrogen. In a joint Edinburgh-Porto (Paula Tamagnini) initiative, they reported for the first time the investigation of a non-heterocystous filamentous cyanobacterial species, targeting hydrogenases using molecular techniques. This initiative was facilitated through meeting contact at the IE A Annex 15 ExpertsMeeting in (Germany) 2000.

Initially, primers constructed against conserved regions within hydrogenases from Anabaena sp. PCC 7120 (uptake hydrogenase) and Anabaena variabilis (bi­directional hydrogenase) were used. Once preliminary sequences were analysed, Lyngbya majuscula specific primers were developed to obtain contiguous sequences. Their studies have shown that Lyngbya majuscula CCAP 1446/4 contains both the hupS and hupL genes encoding the small and large sub-unit of the uptake hydrogenase. Additionally, the hoxY gene (small sub-unit of the hydrogenase moiety) of the bi-directional enzyme was also sequenced. To date, they have obtained a 3 kb segment corresponding to a vast majority of the hupS and hupL gene, including an intergenic region of 643 bp. The HupS and HupL proteins are -80% identical (90% similar) to the corresponding proteins in the filamentous heterocystous strains Nostoc punctiforme (PCC 73102), Anabaena variabilis, and Anabaena PCC 7120. A fragment of approximately 300 bp within the hoxY gene was also sequenced.

Preliminary physiological studies are currently underway to determine the pattern of nitrogenase and hydrogen uptake activities present within Lyngbya majuscula CCAP 1446/4.

As a future lead to a biotechnological process, successful studies were carried out at 0.25 to 250 litre scale whereby, a stable and viable biomass of Lyngbya majuscula CCAP 1446/4 was achieved allowing long-term harvesting for over 12 months.

F) Present Biohydrogen activities in Norway (Torsten Kallqvist)

The new Biohydrogen project, recently funded by the Norwegian research Council was presented and discussed. This five years initiative will include both green algea and cyanobacteria and will span from molecular biology to more applied bioreactor studies. Several universities and NIVA will be partners in this joint effort.

G) Present Biohydrogen activities in Portugal (Paula Tamagnini)

9.9-

In addition to the molecular characterizations of cyanobacterial hydrogenases in Porto, the molecular structure of the hydrogenadse of D. gigas is being analyzed in Lisbon (Moura) and the overall protein chemistry of the Pyrococus hydrogenase in Porto.

Concentrating on the unicellular cyanobacterium Gloeothece ATCC 27152, the initiative in Porto has cloned and sequenced part of the one copy genes hupSL and confirmed the absence of structural genes encoding a bidirectional enzyme. Moreover, the uptake hydrogenase activity follows the nitrogenase activity.

E) Present Biohydrogen activities in Sweden (Peter Lindblad)

The molecular characterization of cyanobacterial hydrogenases has continued. An up-to-date description of the present knowledge about both the uptake hydrogenase and the bidirectional enzyme was presented. Through a specific cooperation between Sweden and Portugal, a detailed overview has been compiled, at present submitted for publication in a leading international journal;

Cyanobacterial Hydrogenases (Tamagnini, Axelsson, Lindberg, Oxelfelt Wunschiers & Lindblad). Summary: Cyanobacteria may possess several enzymes directly involved in dihydrogen metabolism: nitrogenase(s) catalyzing the production of hydrogen concomitantly with the reduction of dinitrogen to ammonia, an uptake hydrogenase (encoded by hupSL), catalyzing the consumption of hydrogen produced by the nitrogenase, and a bidirectional hydrogenase (encoded by hoxFUYH), which has the capacity to both take up and produce hydrogen. This review summarizes our knowledge about cyanobacterial hydrogenases focusing on recent progress since the first molecular information was published in 1995. It presents the molecular knowledge about cyanobacterial hupSL and hoxFUYH, their corresponding gene products, and accessory genes before finishing with an applied aspect - the use of cyanobacteria in a biological, renewable production of the future energy carrier molecular hydrogen. In addition to scientific publications, information from three cyanobacterial genomes, the unicellular Synechocystis PCC 6803, and the filamentous heterocystous Anabaena PCC 7120 and Nostoc punctiforme (PCC 73102/ATCC29133) is included.

Initial bioreactor experiments, using wildtyp and genetically modified strains were presented. E.g. a mutant with the gene encoding the uptake hydrogenase inactivated evolves molecular hydrogen at a similar rate as the sulfur deprived green algae discussed above. Moreover, a method for examinig "real competition experiments" between different strains, e.g. wildtype and mutant, was presented and discusseed.

IN SUMMARY, real progress is presently being done within all four subtasks;

A - Genetic information of both cyanobacterial and green algal hdyrogenases,B - Reducing the antennna size complexes,C - Fermentations, and D - Bioreactor systems.

1.2. International exchange

Several putative scientific exchanges were identified during the ExpertsMeeting. In addition, several of the participating laboratories are continously exchanging ideas, suggestions, comments etc etc improving the overall scientific outputs within the respective projects.

1.3. Presentations of Annex 15

During 2000, Annex 15 was presented at several international meetings, resulting in two publications which will be used as references when publishing, presenting, discussing biohydrogen in general as well as the specific biohydrogen activitis in the respective individual laboratories;

* Lindblad, P., Asada, Y., Benemann, J., Hallenbeck, P., Melis, A., Miyake, J.,Seibert, M. and Skulberg, 0. 2000. IEA Hydrogen Agreement, Task 15:Photobiological Hydrogen Production - An International Collaboration. Hydrogen Energy Progress XIII. Volume 1: 56-59. Editors: Mao, Z.Q. and Veziroglu, T.N.

* Lindblad, P., Asada, Y., Benemann, J., Hallenbeck, P., Melis, A., Miyake, J.,Seibert, M. and Skulberg, O. 2000. IEA Hydrogen Agreement, Task 15:Photobiological Hydrogen Production - An International Collaboration. Proceedings 10th Canadian Hydrogen Conference. Pages: 731-733. Editors: Bose, T.K and Benard, P. ISBN 0-9696869-5-1.

1.4. Extension of Annex 15

The extension of Annex 15 after the initial 3 years has been discussed. Both the countries that joined Annex 15 in the beginning and those joining later or being in a process of signing Annex 15 would like to both continue and to expand this most fruitful cooperation. It was agreed to circulate the present description of Annex 15 with the aim of discussing the specific text for the extension at the next ExpertsMeeting in September 2001 followed by a discussion at the ExCom meeting in October 2001.

1.5. New members

Many contacts have been taken during the last 6 months. Outcome'. The Netherlands and UK are close to joining Annex 15. Experts from Hungary, Italy and Portugal are participating with discussions with the respective governments on the process of joining. Mexico has expressed an interest to join and China has outlined most relevant activities for annex 15.

1.6. BioHydrogen 2002

The International BioHydrogen 2002 conference was discussed during the Experts Meeting. The suggestion is an international BioHydrogen conference to be held in The Netherlands in April 2002. This will be organized together with a meeting of COST action 8.41 - Biological and Biochemical Diversity of Hydrogen Metabolism), specifically working group 4 (Biohydrogen).

The overall possibilities of joining forces with COST 8.41 was also discussed and as ONE outcome. The next Experts Meeting will be held jointly in Hungary (Szeged) in September 2001.

2. Work Plan for the Next Six Months

2.1. Continue to work on increasing the number of participating countries actually signing Annex 15.

2.2 Initiate a detailed discussion (alredy initiated at the last ExpertMeeting) on goals and strategeis for the years 4 and 5 of Annex 15.

2.3. Organize the international conference BioHydrogen 2002

2.4. • Summarize performances by a genetically modified mircoorganismin a small scale bioreactor, including competition experiments

• Perform fermentaion experiments using different systems and organismswith the aim of comparing and evaluating organisms, systems, yields etc etc

• Initiate calculations of the efficiencies of hydrogen production by bothcyanobacteria green algae

• Summarize the knowledge of cyanobacterial fermentations

2.4. Next Experts-Meeting are planned to be held in Hungary (Szeged; September 10-11, 2001), and The Netherlands (April 2002; BioHydrogen 2002).

3. Matters requiring ExCo attention

• Advice on how to proceed with the putative new IEA Hydrogen Agreement members Hungary, UK, Portugal, Mexico and China

Hungary - A meeting is scheduled between a Hungarian Governmental representative, the suggested Exert (Kovacs) and the OA for July 6.

UK - Most relevant activities have been identified and the suggested Expert (Wright) has participated in the last two experts meetings.

Portugal - A detailed letter explaining the procedure of joining is needed.

Mexico & China - More information is needed.

• Allocate economical resources from the common fund to support the international conference BioHydrogen 2002. Dollars are needed for the initial organization, to invite some selected speakers, for some common activities during the conference, and to handle and publish the present status of Biohydrogen as a special issue of an international journal.

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Appendix 1

IE A Hydrogen Agreement Annex 15 ExpertsMeeting March 26-27, 2001

Porto, Portugal

1. Opening.

2. Presentations of present/recent activities in participating

laboratories & countries.

3. Continuation of Annex 15. Short term & long term.

4. BioHydrogen 2002 - An international conference.

Decision; Place, Dates, Organization & Publication.

5. Cooperations & Exchanges within Annex 15.

6. Final Report Annex 10B.

7. Future ExpertsMeetings.

8. Closing.

— 33 -

Appendix 2

Microalgae: A green source of renewable H2

TIBTECHDecember 2000 volume 18: 506-511

Ghirardi et al / USA

Attached as a separate pdf-file

IEA Hydrogen Implementing Agreement

Annex 17 - Solid and Liquid State Hydrogen Storage Materials

Action Items for May, 2001, Executive Committee Meeting

Transmittal of Charter Project Plans

Date: 9 April 2001

From: Gary Sandrock, Operating Agent (sandrock@warwick.net)

To: Task 17 Participating ExCo Members Canada (N. Beck)Iceland (TBD - ad hoc D. Haberman)Israel (TBD - ad hoc D. Haberman)Japan (T. Abe)Mexico (J. Sebastian)Norway (T. Riis)Sw eden (K. von Kronhelm)Switzerland (G. Schriber)United Kingdom (R. Eaton)United States (N. Rossmeissl)

CC: All other ExCo Members, Y. Tsuji, D. Haberman

1. Overall Status of the Task

As per the instructions of the ExCo (Madrid Minutes 3.2), I have worked with all the potential Task 17 Experts to create a structured spectrum of charter projects. This effort is virtually complete and is shown in the following Status Table. At its completion, Task 17 will consist of approximately 10 countries, 28 lead organizations, 28 projects and a total level of effort of at least 17 person-years/year. I shall ask for the approval of at least 23 of these projects at The Hague ExCo Meeting, thus formally initiating the Task and starting the 3-year clock.

2. Project Spectrum and Status

The participating countries, lead organizations, project leaders, proposed levels of effort, project titles and project numbers are summarized in the attached 2-page tabular summary. Plans for the 23 projects listed in black have been submitted and are all attached to this memo. The three entries listed in red are promised, but have not been received as of this date. (In order to give you adequate time to review the many Project Plans, I have elected to forward what I have now; the remaining three will be forwarded when received). Finally, the two projects listed in blue represent the newest Task 17 applicants, Iceland and Israel. These two countries have not yet formally joined IEA H2, but their involvement is anticipated.

The spectrum of participants and projects represents an unprecedented international consortium of hydrogen storage activities. Projects range from the highly fundamental to the practical. They include experimental, theoretical, modeling and engineering activities. The projects are divided into three categories: hydride only (H-l to H-11), carbon only (C-l to C-4) and hydride plus carbon (HC-1 to HC-8). It is requested that the attached Project Plan information be kept CONFIDENTIAL for the near future and not be distributed outside IEA H2.

There are some minor overlaps and duplications of effort among the various projects. However, I am not concerned by this fact. Competition in the storage area is good; duplications of results are critical and much needed in certain areas. But in a larger sense, personal interactions among the Experts will result in the ultimate elimination of duplications, thus resulting in more efficient utilization of R&D funds.

3. Approval of the Charter Projects

I hereby request and recommend approval of the 23 Project Plans attached to this memo (as well as any others that may be transmitted before the ExCo Meeting). Because of time limitations, I will not present individual projects at the meeting, but will be prepared to answer questions any ExCo Member may have before the votes are

IEA Task 17 (9 April 2001)

— —

taken. All participating Task 17 ExCo members will be asked to vote; those not able to attend The Hague meeting are asked to submit their votes in writing to the Executive Secretary (in advance of the Meeting).

4. Waiver of Minimum Participation Level for Mexico

As approved by the ExCo at Madrid, the official minimum national participation for Task 17 is 1.0 person- year/year. Mexico’s proposed participation is 0.3 py/y (see Project HC-2), i.e., below that minimum. I hereby request ExCo approval to waive the minimum participation level for Mexico.

5. National Participation Letters

As per the instructions of the ExCo (Madrid Minutes 3.2), I shall prepare draft National Participation Letters for each of the Task 17 participating ExCo Members. These letters will be consistent with the final levels of effort indicated by the Project Plans. I shall include the names of the lead Experts, including both those individuals funded by ExCo Members’ organizations and those funded by other sources (e.g., defense department, corporate or other funding sources). However, in view of the fact ExCo Members usually cannot legally commit Experts they do not fund directly, non-ExCo-Experts will be marked with a qualifier “for information only”. At the present time, I do not plan to obtain separate binding Participation Letters for the non-ExCo-Experts. Rather, I will ask the ExCo at The Hague if they wish me to obtain such Letters in all cases, or alternatively “trust” those participants to serve in good faith according to the IEA H2 rules.

6. Other Business

The above covers the Task 17 business anticipated at the upcoming The Hague ExCo Meeting. I shall inform you if any other items of business should appear. Alternatively, any ExCo Member should feel free to contact me on any matter relating to the Task, or anything I have missed at this time.

Respectively submitted 9 April 2001 Gary Sandrock, Operating Agent

Attachments:Participation Status Table (2 pages)Project Plans (H-l to H-l 1; C-l to C-4; HC-1 to HC-8)

IEA Task 17(9 April 2001)

IEA Hydrogen Implementing Agreement

Annex 17 - Solid and Liquid State Hydrogen Storage Materials

Participation Status Table (as of 9 April 2001)

Status Color Codes:

Project Plan received (black)Project Plan expected, but not yet received (red) Participation still in discussion stage (blue)

TBD = To be decided

Country Institution Proj. Leader Effort Title or Subject Proj.#

Canada HRI-UQTR R. Chahine 0.3 Hydrogen Storage in Single-Wall Carbon Nanotubes

C-l

Canada Hydro-Quebec J. Huot 0.5 Real time synchrotron studies of hydrides H-2Canada McGill U. A. Zaluska ? Lithium-beryllium hydrides —

Iceland 1 B D 1 BD 9 Hi removal from geothermal gases (?) —

Israel Bcn-Gurion U. M. Mintz 7 Metal hydride electrodes (?) -

Japan Kogakuin U. S. Suda 1.5 Alkaline borohydride solutions as El- generation system

H-3

Japan EERI-NIAIST E. Akiba 1.0 Zintl phase hydrogen absorbing compounds H-4Japan GLT-NIAIST N. Kuriyama 1.0 Research of new X-TM-Y alloys (X=Ca,

Mg, Li; TM=transition metals; Y=metals)H-5

Japan Hiroshima U. H. Fujii 0.5 H-storage in nano-structured carbon-related materials and hydrides

HC-1

Mexico CIE-UNAM S. Gamboa 0.3 Hydrogen storage in metal hydrides, nanotubes and carbon

HC-2

Norway 1FE B. Hauback 0.5 Structural characterization of hydrogen storage materials

HC-3

Norway IFE V. Yartys 0.5 Nonconventional hydrides with low H-H separations

H-6

Norway Norsk Hydro C. Rosenkilde 0.5 Kinetics of hydrogen release and uptake HC-4Sweden Stockholms U. D. Noreus 1.0 Destabilisation of hydrides based on hydrido

complexesH-7

Switzerland U. of Fribourg A. Ziittel 1.0 H-storage in nanostructured carbon and metals

HC-5

Switzerland U. of Geneva K. Yvon 3.0 Destabilization of metal hydride complexes and theoretical modeling

H-8

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IEA Task 17 (9 April 2001)

IEA Hydrogen Implementing Agreement

Annex 17 - Solid and Liquid State Hydrogen Storage Materials

Participation Status Table (as of 9 April 2001)

(concluded from previous page)

Country Institution Prop Leader Effort Title or Subject Pro).#

IK DURA B. Lake-man ? Hydrides and carbon for hydrogen storage -

UK U. of Bath T. Mays 1.0 Hydrogen storage in carbon nanotubes C-2UK U. of

StrathclydeP. Hall 1.25 High Pressure X-Ray Diffraction

Measurements of Hydrogen in Nano- structured Carbon

C-3

UK BirminghamU.

J. Speight 1.0 FUCHSIA: Fuel Cell and Hydrogen Store for Integration into Automobiles

HC-6

UK Li. of Salford K. Ross(?) ? ■>USA Ergenics, Inc. D. DaCosta 0.2 Thermal Hydrogen Compression with

PurificationH-9

USA MER Corp. R. Loutfy 0.3 Feasibility of fullerene hydrides for high capacity hydrogen storage applications

C-4

USA NREL M. Heben 0.3 Hydrogen: Storage in Single-Wall Carbon Nanotubes

C-l

USA NRL A. Imam 0.5 Development and Characterization of Advanced Materials for Hydrogen Storage

HC-7

USA Sandia NL K. Gross 1.0 Catalytically modified hydriding properties of novel complex hydrides

H-10

USA Sandia NL G. Thomas 0.25 Engineering Properties of New Storage Materials

HC-8

USA SunaTech, Inc. G. Sandrock 0.3 IEA/DOE/SNL hydride databases H-lUSA U. Hawaii C. Jensen 1.5 Solid State Nuclear Magnetic Resonance

Spectroscopic Studies of Catalytically Enhanced Sodium Aluminum Hydride

H-l 1

IEA Task 17 (9 April 2001)

Project No. H-l

Title: IEA/DOE/SNL on-line hydride databases

Project Leader: G. Sandrock (SunaTech, Inc.) - USA Type of Project: ReviewInternational Collaborations: S. Mitrokhin (Lomonosov Moscow State U.) - Russia Level of Effort (Duration): 0.3 py/y (3 years)

BackgroundThis Project had its origins in IEA Task 12. As an effort to aid Task 12 Experts in defining and

executing their R&D efforts, an extensive hydride literature review was commissioned. It was quickly decided to share the results of this effort with all interested parties. Therefore a series of comprehensive hydride databases were constructed and made freely available on the rapidly expanding Internet (URL http://hydpark.ca.sandia.gov). They include extensive listings of alloys reported to hydride, detailed engineering properties on selected hydrogen storage elements and alloys, a hydride applications database and a large reference list. In addition, an M-H organizations list and M-H meetings calendar have been included. These databases have evolved into an important international information reservoir to hydride scientists and engineers. Typically the website experiences about 20 hits per day.

It is proposed that the database effort be continued throughout the duration of Task 17. We need to continue updating of the existing databases, as well as create new ones. In particular, we need to seriously consider the addition of a database on carbons as H2 storage media.

Project PlansG. Sandrock will continue to review the English, Gennan and French literature and update the

existing databases. He will be assisted by S. Mitrokhin, who will search the Russian-language hydride literature (past and current). G. Thomas (Sandia Consultant) will continue to be responsible for the website server and any associated hardware and software problems therewith.

The hydride databases have been seriously neglected since late 1999. The first priority will be updating recent literature, as well as including some of the missing Russian literature. There is need to create a new (Miscellaneous) hydride database to include such diverse materials as amorphous, nanocrystalline, multiphase, quasicrystalline, etc. We will also consult with the carbon Task 17 Experts for advice if and how we should create a C-H database and reference list. Consideration will be given to the possible creation of a electrochemical hydride database, but at best this would be added late in the Task. When the existing databases are updated and the new ones formed, we plan to publish the entire series in the form of a searchable CD.

Milestones

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Milestone Month/Y earStart identification of Russian-language literature 05/01Complete retrospective update of existing hydride databases 12/01Complete Miscellaneous hydride database and put on-line 05/02Go/no-go decision on Carbon-Hydrogen database 05/02Complete C-H database (if “go” above) 10/02Publish all databases in CD-ROM form 07/03Final database updates before end of Task 05/04

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IEA Hydrogen Implementing AgreementAnnex 17- Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-2

Title: Real time synchrotron studies of metal hydrides

Project Leader: J. Huot (Hydro-Quebec) - CANADAType of Project: ExperimentalInternational Collaborations: TBD (in negotiation)Level of Effort (Duration): 0.5 py/y (3 years)

BackgroundThis project originates from a study we did on MgH2-Nb nanocomposites. This system has very fast

hydrogen sorption properties but the exact mechanism of how the hydrogen goes in and out is not fully understood. Because of the very fast hydrogen sorption kinetics, real-time in-situ structural studies using conventional diffractometers were impossible. Therefore, we investigated the sorption mechanism by using X-ray synchrotron powder diffraction measurements that provide very high photon flux. In this experiment, a complete diffraction pattern could be perfonned in 5 ms.

In the first experiment on MgH2-Nb nanocomposite, only the hydrogen desorption process was investigated. We found that a metastable niobium hydride phase acts as a gateway though which hydrogen released from MgH2 flows.

The efficiency of this technique having been proved, it could now be used to investigate other metal hydride systems to have a better understanding of the hydrogen sorption mechanism.

Project PlansMost of the work will be perform by a post-doc candidate. First, we will use the present (or slightly

modified) sample cell for measuring the desorption process in various metal hydrides (low, medium and high temperature) doped with different additives. The objective of this first phase of the project is to study the hydrogen desorption mechanism in different hydrides and to acquire experience with the real­time synchrotron X-ray diffraction technique.

In the second phase of the project, we will build a dedicated sample cell for studying absorption processes. This means that the cell should be able to work under high hydrogen pressure and high temperature.

MilestonesBecause this project involves large equipment (synchrotron) that could not be accessed on a day

to day basis, we prefer to mention only a few milestones. The actual progress may be faster than this, depending on the level of availability of the synchrotron.

Milestone Month/YearMeasurement of desorption process in metal hydrides 12/01Design, fabrication and testing of pressurized sample holder 08/02Measurement of absorption process in metal hydrides 06/03

IEA Task 17 (9 April 2001)

— <4.0 —

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-3

Title: Alkaline borohydride solutions as H-generation system

Project Leader: S. Suda (Kogakuin University) - JAPAN Type of Project: Experimental, Engineering International Collaborations: Not available Level of Effort (Duration): 1.5 py/y (3 years)

BackgroundUnavailable

Project PlansAims: (1) To develop H-storage and supply systems for PEM Fuel cells, and (2) To establish a production and recycling process that applies Borax as the natural resource and Borates as the recyclable fuel sources.Phase-1(a) To develop catalysts for the hydrolysis of Borohydride solutions.(b) To design and construct a demonstration reactor.(c) To demonstrate the highest attainable H-generation rate of 16.8 liters/s (1.5g/s).(d) To design plate types of catalyst with larger surface area that is consisted by the fluorinated Mg- hydrides.Phase-2(a) To develop a venti-scale production process for KBH4 and NaBH4 both from Borax and Borates.(b) To develop a pilot-scale production process for KBH4 and NaBH4 both from Borax and Borates.(c) To develop the fluorination technique for preparing partially hydrided Mg.

Milestones

Unavailable.

IEA Task 17 (9 April 2001)

— A 1 —

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-4

Title: Zintl phase hydrogen absorbing compounds

Project Leader: E. Akiba: Energy Electronics Research Institute, National Institute of Advanced Industrial Science and Technology - JAPAN Type of Project: ExperimentalInternational Collaborations: Under consideration (with expected Task 17 participants)Level of Effort: 1.0 py/y (3 years)

BackgroundAlanates have higher hydrogen capacity than interstitial hydrides in general and metal-

hydrogen bonding in alanates is covalent. However, alanates in the solid fonn are explosive and are synthesized by chemical process. Interstitial hydrides are directly synthesized using hydrogen gas and intermetallic compounds. We found a new class of intermetallic compound, the Zintl phase. The hydride of Zintl phase is synthesized by the same process to interstitial hydrides and has metal-hydrogen covalent bonding that presumably makes hydrogen capacity higher than that of interstitial hydrides.

Project PlanWe have two sub-subjects in this program; one is synthesis of novel Zintl phase compounds

containing A1 and another is investigation of hydrogenation properties of Zintl phase and its hydrides.For synthesis, SrAl2 Zintl compound and its related pseudo-binary compounds will be prepared

by a conventional arc melting method. As the next step, novel Zintl compounds containing A1 will be synthesized using various methods such as ball milling, sintering etc. Hydrogenation properties of these compounds will be investigated and crystal structure that indicates formation of Al-H directly will be carried out.

Milestones Table

5/2001 -5/2002 5/2002 - 5/2003 5/2003 - 5/2004Synthesis of novelZintl compounds

SrAl2 related pseudo­binary compounds

Novel Zintl compound containing A1

Novel Zintl compound containing A1

Investigation of hydrogenation properties of Zintl phase and its hydrides

Determination of hydrogen contents and crystal structure of SrAl2 hydrides

Determination of hydrogen contents and crystal structure of pseudo-binary SrAl2 hydrides

Determination of hydrogen contents and crystal structure of novel Zintl compound containing A1

IEA Task 17(9 April 2001)

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IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-5

Title: Research of new X-TM-Y alloys (X=Ca, Mg, Li; TM=transition metals; Y=metals)

Project Leader: N. Kuriyama (Advanced Industrial Science and Technology) - JAPAN Type of Project: ExperimentalInternational Collaborations: D. Noreus (Stockholm U.)-Sweden, A. Zuttel (Fribourg U.)-Switzerland Level of Effort (Duration): 1.0 py/y (3 years)

BackgroundMetal hydrides are a promising medium for hydrogen storage. However, relatively high cost and

heavy weight of the alloys are the main barriers to their practical use. Intermetallic compounds consisting of Ca and A1 were considered to be one of the candidates for the materials for hydrogen storage because of low material costs and lightweights.

In the Project 4 activities in the Task 12, preparation methods, structural analysis and hydrogenation properties were investigated for CaAl2-based Laves alloys which were modified by the addition of B and Si and for a new CaAlSi alloy which was prepared as a mixture of CaAlSi and CaAl2Si2 phases. During hydrogenation at temperatures higher than 473K, the CaAl2-based and CaAlSi alloys and decomposed to form stable hydrides such as CaH2 and didn’t exhibit reversible hydrogenation behavior.

Taking it into account that some Ca-based compounds such as CaNi5 form their corresponding hydrides, it can be expected that some transition metals such as Ni are necessary as a third element to obtain the Ca-Al-based alloys which can reversibly desorb hydrogen. In the Project 13 activities in the Task 12, ternary Ca-Al-TM (TM; transition metals) alloys were investigated for preparation methods, structural analysis and hydrogenation characteristics. The ternary alloy phase with the compositions of Ca3Al7.xCux (x=3-4) was obtained in a Ca-Al-Cu system. However, this phase did not show reversible hydrogenation behavior, hi Ca-Al-Co and Ca-Al-Ni systems, no new ternary intermetallic compounds were discovered although it was known that there were some ternary compounds, which could form their corresponding hydrides, in RE-Al-Ni systems (RE: rare earth metals).

The objective of this project is to research for the new intermetallic compounds and alloys with the possibility of large hydrogen storage capacities, hi order to find them, phase relations in ternary X- TM-Y systems are mainly investigated, where X and Y mean light and inexpensive metals such as Ca,Mg and Li and other metals, respectively. The ternary intennetallic compounds obtained will be examined for crystallographic structures and hydrogenation characteristics. As well as our Project 13 in the Task 12, this project is exploratory and limited to a preliminary experimental survey on possibilities for gaseous hydrogen storage.

Project PlansH. T. Takeshita (Japan) will make various alloys described above and examine each alloy for

metallographic structures, hydrogenation and dehydrogenation properties andP-C isotherms. Optionally, and if promising results are obtained, D. Noreus (Sweden) and A. Zuttel (Switzerland) will do a structure determination and a treatment for kinetic enhancement, respectively. N. Kuriyama (Japan) and H. T. Takeshita will complete all the data into an IEA report.

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IEA Task 17(9 April 2001)

Project H-5 (concluded)

MilestonesMilestone Month/YearStart selection of hopeful X-TM-Y ternary systems 05/01Choose ternary systems investigated 08/01Start survey of new compounds in Ca-based ternary systems 08/01Complete survey in Ca-based ternary systems 12/02Start survey of new compounds in Mg- and Li-based ternary systems

01/03

Complete survey in Mg- and Li-based ternary systems 12/03Review before end of Task 05/04

EEA Task 17 (9 April 2001)

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-6

Title: Nonconventional metal hydrides with low H-H separations

Project Leader: V. Yartys (Institute for Energy Technology) - NORWAY Type of Project: Experimental International Collaborations: Not specified Level of Effort (Duration): 0.5 py/y (3 years)

BackgroundThe relationship between structure, bonding and hydrogen storage capacities in a principally new type

of metal hydrides capable of reaching H-storage densities several times higher than liquid H2, will be established.

The work will be focused on two aspects:a) characterisation by means of physical methods of the structure, bonding and mobility of hydrogen in the superdense metal hydrides, both binary and intermetallic. These data are necessary to understand better the mechanism of hydrogen-hydrogen interactions in these unusual materials;

b) search for the new advanced materials with the smaller compared to presently found by us limiting value of H-H separations (1.57 A, lowest reported in literature value) and on the extension of the presently reached local hydrogen densities to the bulk behaviour of the metal hydride materials.

Project Plans> Precise structural characterisation of superdense hydrides of titanium and zirconium with use of high-

resolution powder neutron diffraction and synchrotron X-ray diffraction (Swiss-Norwegian Beam Lines, Grenoble). These studies will involve in situ measurements in D2 gas and will provide data concerning site occupancies of H in the metal lattice confirming their superstoichiometry with D(H)/Me » 2.

> High-pressure studies of the evolution of structure and H...H coupling vs. applied pressure in the R3Ni3In3H4 hydrides. Their structures contain pairs of hydrogen atoms with extremely short H-H separations. These range from 1.570(8) to 1.635(8) A, depending on the type of the RE element (powder neutron diffraction data). The volume expansion accompanying hydrogen absorption in RENiln compounds, 7-8 %, is strongly anisotropic and is located to the [001] direction (Ac/c = 15-16 %). We expect that a compression of the metal sublattice of the metal hydride back to the unit cell dimensions of nonhydrogenated alloy would require use of moderate static pressures, probably not exceeding 7 GPa, as compared to high pressure work on another type of metal hydride, YMn2D4. At higher pressures (up to 30 GPa, which we propose to apply) the H-H distances are expected to shrink down to approximately 1.0-1.1 A. Such short H-H separation is close to H-H distance in molecular hydrogen (0.78 A), and an unusual type of both metal-hydrogen and hydrogen-hydrogen bonding is expected at these conditions. Metal matrices containing H atoms coupled into pairs are so far not known. Therefore, it will be very important to study such type of metal hydride. Additional scientific interest is raised by the possibility to synthesise metallic hydrogen with H...H coupling.

MilestonesUnavailable.

IEA Task 17 (9 April 2001)

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IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-7

Title: Destabilisation of hydrides based on hydrido complexes

Project Leader: Dag Noreus (Stockholm University) - SWEDEN Type of Project: Experimental, Theoretical International Collaborations: K. Gross, Sandia NL, USA Level of Effort (Duration): 1.0 py/y (3 years)

Background:Mg2NiH4 is considered to be one of the most promising future hydrogen storage materials. As in

all complex transition metal hydrides the metal-hydrogen bond is very strong and the hydride is thermodynamically too stable to desorb hydrogen at room temperature, hi order to be used in applications, this bond needs to be weakened, which would lead to a more unstable hydride.

The phases and structures of Mg2NiEU have been studied carefully at our University during the last decade and our knowledge about the fundamentals of this hydride is very good. The results are that by disturbing the lattice by doping and disorder the stability as well as other physical properties can be significantly influenced. This work will be extended to first to other nickel-hydrido systems and then later to hydrido complexes based on other metals.

Project Plan:Investigation of metal hydrides based on hydrogen rich transition metal hydrido complexes, in

order to make the stored hydrogen available at lower temperatures. Especially, the bonding and stabilising situation in Mg-Ni hydrides will be used as a reference system when comparing with other hydrides.

Milestones Table:

Year Aim2001 Experimental work, fundamental studies of lattice stabilisation

mechansims of Ni hydrido complexes using different methods.2002 Theoretical work, calculations on energy and bonding in

possible s-element-(Ni-H) configurations. Extension of the work to more general covalent bonded hydrides

2003 Tests of the destabilised hydride as negative electrode in NiMH batteries. Development of non-corroding electrolytes.

IEA Task 17 (9 April 2001)

Project No. H-8

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Title : Destabilisation of metal hydride complexes and theoretical modeling

Project Leader: K. Yvon (University of Geneva) - SWITZERLAND Type of project: Experimental and ModelingInternational Collaboration: Karl Gross, Sandia National Labs, USA Level of effort (Duration): 3 py/y (3 years)

BackgroundDuring the past few years the number of solid-state compounds known to contain transition metal

hydride complexes has dramatically increased. From some twenty compounds about ten years ago there are now over one hundred such compounds known of which half have been discovered in Geneva (1). Their common structural feature is the presence of metal-hydrido anions of which most obey the 18- electron rule. As far as hydrogen storage applications are concerned the most promising candidates are iron based Mg2FeH6 and manganese based Mg3MnH7.

Mg2FeH6 contains octahedral 18-electron [FeH6]4" anions. Its volume efficiency for hydrogen storage (150 g H/litre) exceeds that of liquid hydrogen (71 g H/litre) by a factor of two, and its weight efficiency (5.5 wt.%) meets target A of Task 17. Furthermore, the compound can be fabricated relatively cheaply in large quantities. Although its usefulness for reversible storage of thermal energy at high temperature (~450°C) has been demonstrated, its thermal stability is too high for reversible hydrogen storage applications at room temperature (decomposition temperature at 1 bar hydrogen pressure: ~320°C). Attempts to decrease that stability by partially substituting magnesium by other alkaline earth elements such as calcium resulted in the discovery of new quaternary metal hydrides such as Ca4Mg4Fe3H22. Although the hydrogen storage efficiencies of these compounds were comparable to those of Mg2FeH6, their thermal stability was still too high for reversible hydrogen storage applications near room temperature.

5-Mg3MnH7 contains octahedral 18-electron [MnH6] anions and also has excellent hydrogen

storage efficiencies (119 g H/liter, 5.2 wt.%). However, whilst its thermal stability is significantly lower than that of Mg2FeH6 (the compound starts to decompose already at ~250°C under 1 bar hydrogen pressure into elemental manganese and magnesium) it does not meet target A of task 17.

Project PlanThe present project aims at decreasing the desorption temperature of the complex metal hydrides

Mg2FeH6 and Mg3MnH7 (and of related metal hydrides) along the three following routes. The first attempts to substitute magnesium by divalent metals such as zinc. The latter element is known to be a constituent of complex metal hydrides (i.e. K2ZnH4) and forms a binary hydride that is thermally less stable than binary MgH2. If successful, the substitution is expected to yield quaternary hydrides that are thermally less stable than the ternary ones. The second route consists of testing suitable catalysts to increase the desorption kinetics of Mg2FeH6 and Mg3MnH7 (and of related metal hydrides) at lower temperatures. This will be done in collaboration with K. Gross (Sandia National Laboratories, Livermore, USA). The third route attempts to model the thermodynamic stability of complex metal hydrides by crystal chemistry arguments. No such model exists at present and theoretical calculations of the total energy of complex metal hydrides suffer from a lack of precision given their rather complicated crystal structures. The proposed work consists of modeling the stability of complex metal hydrides in terms of atomic properties such as electronegativity, atomic size and valence electron concentration along similar lines as has been done in the past for other classes of compounds (2,3). There is a large amount of

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A1 —

IEA Task 17(9 April 2001)

Project No. H-8 (concluded)

experimental data available for conventional hydrogen storage compounds such as LaNi5 and derivatives which are used in metal hydride battery applications (some 500 compositions have been reported). Thus it appears that a suitable model should be first developed and tested for these types of compounds and, if successful, extended to the less numerous complex metal hydrides. Based on the results and correlations obtained the conditions of synthesis of metal hydride complexes will be adapted such as to obtain compounds having lower thermal stability. These hydrides are expected to meet target A of task 17 and should definitely open up the class of complex metal hydrides for reversible hydrogen storage applications near room temperature.Milestones Table:Tl year: substitution of magnesium in Mg2FeH6 by zinc; catalyzed desorption experiments on Mg2FeH6 and Mg3MnH7; modeling of LaNi5 type hydrides and derivatives.2nd year: substitution of magnesium in Mg3MnH7 by zinc; catalyzed desorption experiments on substituted Mg2FeH6 and Mg3MnH7; extension of LaNi5 model to complex metal hydrides.3d year: extension of metal substitutions to other complex metal hydrides; application of model to find suitable compositions and synthesis conditions for new (low-stability) metal hydrides; cycling experiments.

1. K. Yvon, Complex Transition-Metal Hydrides, in Advanced Materials in Switzerland, Chimia 52, 613-619 (1998), and references therein.

2. P.Villars, J. Less-Common Met. 102 (1984) 199, and references therein.3. D.G. Pettifor, J. Phys. C: Solid State Phys., 19 (1986) 285, and references therein.

IEA Task 17 (9 April 2001)

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IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-9

Title: Thermal hydrogen compression with purification

Project Leader: D. DaCosta (Ergenics, Inc.) - USA Type of Project: Engineering International Collaborations: None Level of Effort (Duration): 0.2 py/y (2 years)

BackgroundHydrogen produced from renewable energy resources can contain impurities that might interfere with

or do permanent damage to the new, high storage density materials under development, hi addition, some of the newer storage materials absorb hydrogen only at elevated pressure, whereas the hydrogen produced from most renewable energy resources is at or near atmospheric pressure. Traditional mechanical compressors have high capital and installation costs, consume substantial amounts of energy, require frequent maintenance and can add even more contaminants to the hydrogen.

Ergenics is investigating the application of its novel thermal hydrogen compression process to hydrogen produced from renewable resources. The thermal compressor is an absorption-based system that uses the properties of reversible metal hydride alloys. Hydrogen is absorbed into an alloy bed at ambient temperature and is desorbed at elevated pressure when the bed is heated with hot water. Continuous compression is achieved with two identical beds piped in a parallel configuration; one bed is cooled by water and absorbs hydrogen while the other bed is heated with hot water in order to release hydrogen at the same rate. The cool and hot water streams are periodically switched and simple check valves keep hydrogen moving through the thermal compressor.

Previously, reversible metal hydride alloys would sustain damage from hydrogen impurities at low levels of <50 ppm. Ergenics has developed three processes that may permit hydride alloy beds to tolerate higher levels of impurities, in some cases up to 10,000 ppm or more. Passive Purification is used for water vapor and oxygen, Elevated Temperature Desorption is used for CO and CO2, and Automatic Venting can clear inert gas blanketing caused by N2 and CH4. Employing these processes in a thermal compressor may allow simultaneous compression and purification, which resolves two major system- level problems that may be encountered with new, high density storage materials.

Project PlansErgenics will design and build a pilot scale thermal compressor that includes the three purification

techniques and an associated test apparatus. The compressor will be tested on hydrogen containing various inlet impurity levels to determine threshold contamination levels (levels at which compressor performance is affected). Outlet impurity levels will be monitored to determine the effectiveness of compression with purification. Practical results will be correlated with hydrogen purity and absorption requirements of new storage materials.

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IEA Task 17 (9 April 2001)

Project No. H-9 (concluded)

Milestones

Milestone Month/YearStart design effort 05/01Investigate hydrogen inlet requirements for new, high density storage materials

12/01

Build single stage thermal compressor 09/01Build test apparatus 10/01Complete hydrogen-with-impurities test program 06/02Summarize results and conclusions 10/02

IEA Task 17 (9 April 2001)

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-10

Title: Catalytically modified hydriding properties of novel complex hydrides.

Project Leader: K. Gross (Sandia National Laboratories) - USA Type of project: ExperimentalInternational Collaboration: K. Yvon, (Universite de Geneve) - Switzerland Level of effort (Duration): 3 py/y (3 years)

BackgroundThe complex hydrides NaAlH^ and NagAlH^ have demonstrated rapid and reversible hydrogen storage when doped with Ti and other catalysts [1-7]. This model system has provided much of the ground work for catalyst and processing development and continues to give critical insight into the fundamental mechanisms of the catalytically enhanced hydriding processes. However, for practical applications, such as fuel cell vehicles, higher gravimetric storage capacities, as well as better kinetics and thermodynamics are desirable. For this reason we intend to extend our research to other systems of complex hydrides. Many of the complex hydrides known today were discovered by the group of K. Yvon at the University of Geneva [7], Therefore, this work will be pursued through a collaborative effort with the University of Geneva.

Project planSamples of the complex hydrides Mg2FeH6, and MggMnHy and substitutional variants of these hydrideswill be synthesized by the University of Geneva. These will then be doped with Ti-precursor catalysts at Sandia using our current processing methods. Sandia will characterize the thermodynamic and kinetic properties of these materials. Promising results are expected to lead to further refinement of the material processing parameters and long-term cycle tests. Catalyst enhanced reversibility of these and other novel metal hydride complexes could provide the next leap forward in the development of practical hydrogen storage materials.

Milestones:1st year: Catalyzed desorption experiments on Mg2FeH6 and Mg3MnH7, Thermodynamic and kinetics analysis.2nd year: Catalyzed desorption experiments on substituted Mg2FeH6 and Mg3MnH7 Thermodynamic, kinetics, and long-term cycling studies.3d year: Catalyzed desorption experiments on other substituted complex metal hydrides;Thermodynamic, kinetics, and long-term cycling studies.

1. B. Bogdanovic’, M.J. Schwickardi, J. Alloys Comp. 253 1 (1997).2. B. Bogdanovic’, R.A. Brand, A. Marjanovic’, M. Schwikardi, J. Tolle, J. Alloys Comp. 302 36 (2000).3. Gross, K.J., Thomas, G.J., Jensen, C.M., Review paper, MH2000 Noosa, Australia conference proceedings, J.

Alloys and Compounds.4. Gross, K.J., Jensen, C.M., Review paper, Appl. Phys. A 72, 213-219 (2001).5. Gross, K.J., Guthrie, S.E., Takara, S., and Thomas, G.J., J. Alloys and Compounds, 297, 270-281 (2000).6. Sandrock, G., Gross, K.J., Thomas, G.J., submitted to J. Alloys and Compounds.7. Yvon, K., Complex Transition-Metal Hydrides, in Advanced Materials in Switzerland,

Chimia 52,613-619 (1998).

IEA Task 17 (9 April 2001)

— R1 —

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. H-ll

Title: Solid State Nuclear Magnetic Resonance Spectroscopic Studies of Catalytically Enhanced Sodium Aluminum Hydride

Project Leader: Craig Jensen (U. Hawaii) - USA Type of Project: ResearchPotential International Collaborations: I. NMR studies: K. Kumashiro (U. Hawaii) - USA; R, Bowman (Jet Propulsion Laboratory)- USA. II. Complementary inelastic neutron scattering studies: J. Eckert (Los Alamos National Laboratory) - USA. III. Complementary X-ray diffraction studies: K. Gross (Sandia National Laboratory) - USA; N. Kuriyama (Osaka National Laboratory)- Japan Level of Effort (Duration): 1.5 py/y (3 years)

BackgroundRecent studies of catalytic enhancement of sodium aluminum hydride and related saline complex hydrides with selected transition metal dopants have shown that the resulting materials undergo reversible elimination of greater than 4.0 weight percent hydrogen at moderate temperatures through dozens hydrogen discharging/recharging cycles. Despite the remarkable progress that has been made, these materials are unsuitable for practical application as hydrogen earners for onboard PEM fuels cells due to the low rate of the reversible dehydriding of the [A1H6]3" intermediate and the high pressures required for rehydriding. Thus there is a need to developed impvoved catalysts for the reversible dehydriding of sodium aluminum hydride and related compounds. This process would be greatly aided by the identification of the active catalysts in the materials and elucidation of the catalytic mechanism. These goals could possibly be attained through solid state nuclear magnetic resonance (NMR) spectroscopic studies. Towards this end, we have recent developed methods whereby we can directly observe and quantify the different molecular species that are present during the dehydriding and rehydriding of the doped hydrides by solid state 'H, 27A1, and 2-1Na NMR spectroscopy.

Project PlansThe molecular species will be monitored and the species quantified over the course of the dehydriding and rehydriding reactions at reaction temperatures ranging from 80-150 °C. This data will be used to determine the activation parameters for the Al-H bond activation reactions. We also plan to prepare bulk quantities of the catalytically active species through the stoichiometeric reaction of NaAlH4 with the catalyst precursors and characterize them through solid state 'H, 27A1, and/or 23Na NMR spectroscopy. We hope to then determine the identity of the active catalyst through comparison of these spectra to those of authentic samples of titanium and aluminum compounds that are likely catalyst candidates.

MilestonesMilestone Month/Y earDetermine bond activation parameters of Al-H bond in Ti doped

NaAlH4

06/02

Identify active catalyst present Ti doped NaAlH4. 12/02

Elucidation of mechanism of catalytic Al-H bond activation in Ti doped NaAlH4.

05/04

IEA Task 17 (9 April 2001)

R9.—

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. C-l

Title: Hydrogen storage in single-wall carbon nanotubes

Project Leader: M.J. Heben (NREL) - USA Type of Project: ExperimentalInternational Collaborations: R. Chahine (HRI-UQTR) - Canada Level of Effort (Duration): 0.3 py/y (3 years)

BackgroundThis Project aims to develop methods to characterize adsorption of hydrogen on carbon single-wall

nanotubes (SWNT) using the volumetric methods which are familiar to metal hydride researchers. A comparison between hydrogen storage capacities of cut/purified SWNTs measured by temperature programmed desorption and volumetric techniques performed at NREL demonstrates that the two different techniques yield different capacities despite the fact that the accuracy of both techniques has been rigorously confirmed by calibrations based on the decomposition of CaH2, TiH2, and PdH2. Current understanding suggests that the hydrogen capacity, as determined by the volumetric method, is limited by either thermal effects or sample preparation methodologies. The effort proposed here will focus on these two issues to develop methods for performing volumetric capacity assessments of SWNT materials. Since the volumetric method is the default method used by most engineers interested in ascertaining the properties of a hydrogen storage material, the outcome of the project will be quite useful.

Project PlansM.J. Heben and his group at NREL will supply materials to R. Chahine at HRI-UQTR for analysis in his

small-volume, wide-bore volumetric apparatus. Initial work will be done with purified, un-cut SWNT materials. The purified materials will be supplied in annealed and un-annealed forms having different internal surfaces, and different types of tubes. Purified/cut samples will also be supplied for evaluation. In addition to characterization with H2, other probe molecules such as He, Ar, CH4, C02 will also be used to assess possible impact of impurities. Through the course of this project R. Chahine will work with researchers at NREL to incorporate advanced features into the NREL volumetric apparatus.

Milestones Milestone Month/YearDeliver annealed and un-annealed SWNT samples to Chahine 05/01Complete assessment of gas uptake on un-cut samples 12/01

Complete design of wide-bore volumetric system at NREL 05/02Correlate adsorption isotherms and TPD on activated SWNTs 10/02

Relate capacity and impurity tolerance to tube type 07/03Elucidate mechanism and key barriers to deployment 05/04

IEA Task 17 (9 April 2001)

Project No. C-2

Title: Hydrogen storage in carbon nanotubes

Project Leader: T. J. Mays (Department of Chemical Engineering, University of Bath) - UK Type of Project: Experimental / Theoretical / ModellingInternational Collaborations: P.J.M. Carrott (Department of Chemistry, University of Evora) - Portugal Level of Effort (Duration): 1.0 py/y (3 years)

BackgroundCarbon nanotubes are hollow cylinders of carbon with diameters ~mn and lengths -cm.

Nanotubes are typically formed by condensation from hot hydrocarbon vapours, often encouraged by a metal catalyst. The resulting tubes comprise a number of graphene sheets rolled up into concentric cylinders. Typically tube ends comprise hemispherical caps that isolate the central, cylindrical cavity.

There has been an explosion of interest in carbon nanotubes since their discovery in 1991 by Sumio Iijima. One potential application of these materials that has attracted much recent interest is hydrogen storage. A driver for this interest is the environmental benefit of hydrogen as a fuel gas over fossil fuels, in particular reduced CO? emissions. The nanotubes adsorb hydrogen physically both in their central, cylindrical cavities (once the tubes have been opened) and in the interstitial spaces in tube arrays. These adsorption spaces are in the size range corresponding to micropores or small mesopores. Hence adsorption is enhanced compared to larger pores due to the overlap of interaction potentials from opposite pore walls. This enhancement is even greater than in traditional microporous carbons where pore walls are approximately flat.

While the potential of carbon nanotubes as hydrogen storage media has been recognised theoretically, and using computer simulations of adsorption, their practical worth in this application has yet to be proved. The aim of this project is to explore and optimise hydrogen storage in these materials using experimental measurements of adsorption, backed up with predictions from theory and simulations.Project Plans

The project, to be supervised by T.J. Mays, will cover the following key stages: (a) manufacture of carbon nanotubes using a chemical vapour deposition method; this will also include post-treatments to open up tubes by oxidative removal of end caps and shortening tubes (to increase adsorption/desorption rates) by sonication, (b) characterisation of tube structures using optical and electron microscopy, (c) measurements of hydrogen adsorption over a wide range of pressures and temperatures, and (d) theoretical calculations and computer simulations of adsorption to aid interpretation of data from (c). The experimental work will be carried out by a research assistant at Bath; theoretical work and simulations will be carried out by T.J. Mays, and some findamental adsorption characterisation will be carried out in Portugal.Milestones

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Milestone Month/Y earComplete apparatus to make nanotubes 04/02Start adsorption measurements and structural characterisation 04/02Complete initial assessment of hydrogen storage potential 10/02

Start to explore structures to yield optimal storage parameters 10/02

Complete initial optimisation phase 04/03Complete first consolidation period and report 10/03Complete second optimisation phase 04/04Issue final report 10/04

IEA Task 17 (9 April 2001)

— RA —

Project No. C-3

Title: High pressure X-Ray diffraction measurements of hydrogen in nano-structured carbon

Project Leader: Peter J. Hall, University of Strathclyde - UK- Type of Project: Experimental International Collaborations: None Level of Effort (Duration): 1.25 py/y (3 years)

BackgroundThere have been several recent claims of veiy high hydrogen uptake by nano-structured carbon. The

mechanism of uptake is uncertain but theoretical studies have rejected surface uptake and there is speculation that the mechanism involved diffusion between graphitic layers to form a sort of intercalate. There are still questions as to whether the phenomenon exists, to what extent it takes place and how reproducible it is. Part of the explanation for this is that the experimental techniques for monitoring uptake are inadequate. The volumetric technique adopted by Rodriguez et al has serious experimental limitations and the other potential technique, high pressure TGA has questions over buoyancy effects. The whole subject has reached a watershed and what is needed is some unequivocal evidence as to whether intercalated hydrogen really does exist. For this, we propose to use two powerful techniques that will provide this information without any ambiguity: in situ, high-pressure x-ray and neutron diffraction. This is based upon the fact that if hydrogen does indeed diffuse between graphitic layers then there should be some change in the c-axis spacing. Although this could in principal be performed using a conventional diffractometer on a rotating anode source we propose to use synchrotron x-ray radiation in order to obtain the maximum resolution, in case the phenomenon is very subtle, and also to provide real time information during uptake and desorption. We also propose to use neutron diffraction because the scattering cross section of neutrons is similar to that of carbon. This will enable any ordering of hydrogen to be detected. Furthermore, we propose to perform these experiments on samples of nano-structured carbon that have been fully characterised and optimised.Project Plans

Initially we will create fully characterised nano-structured carbon and subject it to exhaustive graphitisation at high temperature and low temperature oxidation to remove any non-graphitizable carbon. Before the high-pressure diffraction techniques our carbons will be tested using electron microscopy and XRD. The high pressure scattering techniques will be performed on the GEM instrument on the ISIS neutron source near Oxford (UK) and the Daresbuiy synchrotron neutron source (UK). The project employs a full time research associate and PhD student.

Milestones

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Milestone Month/YearEstablishment of graphitisation equipment 05/01Initial carbon production 7/01First synchrotron results 08/01First neutron results 10/01Improved carbons produced and tested 10/02Second synchrotron/neutron results 06/02Final carbons produced 04/03Final synchrotron/neutron results 01/04Final thesis/report 09/04

IEA Task 17 (9 April 2001)

— ^ —

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. C-4

Title: Feasibility of fullerene hydrides for high capacity hydrogen storage applications

Project Leader: R. Loutfy (MER Corporation) - USA Type of Project: ResearchInternational Collaborations: S. Klyainkin (Moscow State University) - Russia Level of Effort (Duration): 0.3 py/y (3 years)

Background

Fullerenes are known to form hydrides containing up to 7.7 wt. % hydrogen and, therefore, are promising as an effective light weight and safe hydrogen storage material. Partial reversibility of hydrogenation has been demonstrated by using various catalytic systems, however, more research is needed to understand and identify effective mechanisms of breaking C - H bonds at mild conditions predicted by thermodynamics.

Project Plans

The proposed research will investigate various options of modifying the structure of fullerenes (changing electronic structure by doping with electron-donating foreign atoms, structural fragmentation, engineering specific catalysts, etc.) to improve their ability to release hydrogen under mild conditions to provide the overall hydrogen storage capacity in the range of 5.5 - 6.0 wt.%.

Milestones

Milestone Month/YearSummarize previous knowledge on fullerene-doped compounds 09/01Prepare, characterize and evaluate samples of doped fullerenes 04/02Investigate cage fragmentation effect on hydrogen storage 06/02Investigate doping effect in conjunction with catalyst 12/02Select and optimize fullerene system 06/03Publish data 05/04

IEA Task 17 (9 April 2001)

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. HC-1

Title: H-Storages in nano-structured carbon-related materials and hydrides

Project Leader: H. Fujii (Hiroshima Univ.) - Japan Type of Project: Experimental International Collaborations: Not specified Level of Effort (Duration): 0.5 py/y (3 years)

BackgroundThis Project is on the base of a Proposal-based New Industry Creative-type Technology R&D

Promotion Program from NEDO, an Industrial Technology Research Grant Program from NEDO and a Scientific Research on Priority Area A of ‘New Protium Functions’ from the Ministry of Education, Science and Culture, Japan. In the above three projects, we proposed three key words of nano-structure, amorphous and nano-composite for developing high-performance hydrogen storage materials. We expect to extract excellent hydrogen storage properties in nano-structured, amorphous or nano-composite materials using cooperative phenomena that hydrogen exhibits in nano-scaled grain boundaries or nano- scaled composite boundaries. Recently, nano-structured graphite was prepared by a mechanical milling technique under a hydrogen gas pressure of 1 MPa. We found that the hydrogen concentration estimated by oxygen-combustion analysis and by thermal desorption mass-spectroscopy reached up to 7.4 mass% (CH0 95). On the other hand, multi-layered Pd/Mg thin films were prepared by an R.F. associated magnetron sputtering method to clarify whether the cooperative phenomena are realized in nano­composite alloys. The results indicated that Mg film absorbed hydrogen up to 5 to 6 mass% and the hydrogen desorbed at 360 K, suggesting that the cooperative phenomenon is realized in nano-composite thin film alloys in which the thickness of the films was well controlled to nano-sizes..

Project PlansS. Orimo will at first study to clarify hydrogen storage properties in nano-structured graphite prepared

by mechanical milling technique, especially the desorption process. After the clarification, he plans to investigate how to improve the hydrogen desorption process. He will be assisted by P. Wang, who will charge the study of additional metal effects in graphite on hydrogen storage properties.

H. Fujii will continue to study hydrogen storage properties in nano-composite thin films to know how to extract some advantageous storage properties in composite alloys. He will feed back the concept of cooperative phenomena in thin films into powder techniques for developing bulk materials. He will be assisted by D. Chen, who will search Mg-based new nano-composites as suitable hydrogen storage materials by the sputtering method. Later, he will try to make them into bulky materials for hydrogen storage as well. H. Fujii will be responsible for the above two projects and give some suggestion in experimental problems that will meet herewith.

(continued on next page)

IEA Task 17 (9 April 2001)

— R7 —

Project No. HC-1 (concluded)

MilestonesMilestone Month/YearStart clarification of hydrogen storage properties in nano-graphite 05/01Start additional effects on hydrogen storage properties 10/01

Confirm cooperative phenomena that hydrogen shows in nano­composite Mg-based alloys

11/01

Complete the additional effects in graphite 05/02Start searching studies of new nano-composite Mg-based alloys 10/02

Feed back the concept of cooperative hydrogenation into powder process

07/03

Clarify final conclusion to the goal before end of Task 05/04

IEA Task 17 (9 April 2001)

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Project No. HC-2

Title: Hydrogen storage in metal hydrides, nanotubes and carbon

Project Leader: S.A. Gamboa/P.J. Sebastian, CIE-UNAM, Temixco, Morelos, Mexico; J.A. Chavez, IIM-UNAM, Circuito Exterior, C.U., D.F. Mexico Type of Project: Experimental and TheoreticalInternational Collaborations: Dr. D O. Northwood/Dr. M. Geng, University of Windsor, Windsor, Ontario, Canada; Prof. Allen Hermann, University of Colorado, Boulder, Colorado, USA Level of Effort (Duration): 0.3 py/y (3 years)Background

This new project has its origin in another recent project on modern batteries (metal hydride and Li- ion). The modem battery project is still an ongoing project in the two institutes of UN AM (Energy Research Center, Temixco and Materials Research Institute, Mexico City). There is a strong interaction in the metal hydride battery area with Dr. Northwood's group in Windsor, Canada. The major collaboration in this area is concentrated in the study of charge/discharge mechanisms in metal hydrides, characterization of the metal hydride/electrolyte interface by employing electrochemical as well as solid state impedance spectroscopy techniques. We have also done simulation studies of the electrochemical impedance spectra as electrical equivalent circuits to characterize the electrode/electrolyte interface. Prof. Hermann has done studies on Pd-nanotube incorporated negative electrodes for MH-batteries.

The project on Li-ion batteries are mainly concentrated on developing new electrode materials (positive as well as negative) and solid state electrolytes for high energy density, power density, longer life and compact batteries. It is proposed that the ongoing studies in metal hydride and Li-ion batteries be continued throughout the duration of Task 17.Project Plans

S. Gamboa (CIE-UNAM) will concentrate on metal hydride hydrogen storage, simulation of equivalent circuits that correspond to electrochemical impedance spectra, charge/discharge mechanisms in electrochemical hydrogen storage and also metal hydride batteries. J.A. Chavez (IIM-UNAM) will be studying the solid state electrolyte for metal hydride as well as Li-ion batteries and solid state impedance spectroscopy and Ritveld method to characterize the electrolytes. D. Northwood and Dr. M. Geng (Univ. of Windsor) continue on the electrochemical charge/discharge mechanisms of metal hydrides. Prof. Hermann (Univ. Colorado) will synthesize and characterize nanotubes for electrochemical hydrogen storage. P.J. Sebastian (CIE-UNAM) will be coordinating the activities on Li-ion batteries, electrochemical hydrogen storage in nanotubes and different forms of carbon (nanotubes, fullerens). Milestones

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Milestone Month/Y earIdentification of suitable metal hydrides, nanotubes & different forms of carbon for hydrogen storage

06/01

Compile the database on existing literature on hydrogen storage in metal hydride, nanotubes & different forms of carbon

12/01

Electrochemical charge/discharge of hydrogen in metal hydrides 06/02Simulation of equivalent circuits corresponding to electrochemical impedance spectra

06/02

Electrochemical charge/discharge of hydrogen in nanotubes 12/02

Electrochemical hydrogen storage studies in fullerenes 06/03Final report on electrochemical hydrogen storage 05/04

IEA Task 17(9 April 2001)

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. HC-3

Title: Structural characterization of hydrogen storage materials

Project Leader: B. C. Hauback (Physics Department, Institute for Energy Technology) - Norway Type of Project: ExperimentalInternational Collaborations: Collaborators in Russia, Ukraine, Sweden, France etc.Level of Effort (Duration): 0.5 py/y (3 years)

BackgroundThe Physics Department at Institute for Energy Technology (LFE) has been involved in

fundamental studies on hydrogen storage materials for several decades, and during the last years the focus has been on synthesis and structural characterization of new metal hydrides. In addition, the Physics Department is responsible for the neutron-based materials research in Norway using the research reactor JEEP II located at DFE. Thus, the combination of broad expertise in neutron scattering and basic knowledge of structure-property relationships in hydrogen storage materials is important for our participation in Annex 17. In particular the high-resolution powder neutron diffractometer, PUS, is important for studies of hydrogen storage materials. We also possess a broad expertise in X-ray scattering techniques (including synchrotron radiation) in general, and use both standard and synchrotron X-ray diffraction routinely in our research. By an Adjust Professor position at the University of Oslo (Hauback), we have direct access to very modem electron microscopes (TEM/SEM). Standard equipment for sample preparation and thermal analysis is available in our laboratory.

Project PlansThe use of neutron scattering is a very important tool for structural characterization of hydrogen

storage materials, both for metal hydrides and carbon-based materials. The powder diffractometer PUS can be used for experiments at temperatures between 7 and about 1400 K. hi addition an in-situ cell optimized for hydrogen/deuterium is available for experiments up to 10 bar pressure and 1400 K. Our contribution to the project will be on structural characterizations using different scattering techniques: mainly neutron scattering, but also X-ray and electron diffraction/microscopy. We will concentrate our own research on different types of advanced metal hydrides, both materials based on light elements and materials with possible enhanced hydrogen density, hi addition we will contribute to the other partners of the IEA Annex 17 on structural characterizations (including neutron in-situ experiments) of different types of advanced hydrides and carbon-based materials.

MilestonesMilestone Month/yearDefine own project to be included in the Task 17 06/01Establish collaboration projects 12/01

Report progress structural work 06/02Report progress structural work 12/02

Report progress structural work 06/03Report progress structural work 12/03Final report of Task 05/04

IEA Task 17 (9 April 2001)

— AH —

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. HC-4

Title: Kinetics of hydrogen release and uptake

Project Leader: C. Rosenkilde (Norsk Hydro ASA) - Norway Type of Project: Experimental, modelling International Collaborations: Not specified Level of Effort: 0.5 py/y

BackgroundNorsk Hydro has a strong tradition in hydrogen production, and was the world’s largest producer of

hydrogen in the 1950ies, at that time by water electrolysis. Norsk Hydro is still a large producer of commercial water electrolysers. Large amounts of H2 are produced also today, but now mainly from fossil fuels. The hydrogen is produced on site and used in our fertiliser plants world wide.

Fossil fuels are expected to be the primary source of hydrogen in the first stages of the hydrogen society. Norsk Hydro is also a large oil and gas producer on the Norwegian continental shelf. This, together with our hydrogen knowledge, places us in a good position to become a significant player in the hydrogen society.

An important aspect of hydrogen storage materials is of course the amount of hydrogen they can store, but equally important is their ability to release and take up hydrogen in a reasonable time. This time is for many of the promising storage materials strongly linked to the catalytic properties of the material.

At the research centre in Porsgmnn, Norway, there is a strong and well-equipped group working with catalysis, both for the petrochemical and fertiliser industry. This group will be able to study the kinetics of hydrogen uptake and release in different hydrogen storage materials. Together with common analytical techniques such as SEM and XRD, the results should form a basis for description of the catalytic properties of the materials and hopefully bring forward methods to improve rates of hydrogen uptake and release.

Project PlansNorsk Hydro will not produce hydrogen storage materials ourselves, and must therefore rely on

supply from other sources. Some material is available from IFE in Norway, such as metal hydrides and carbon materials. We also hope to receive samples for testing from some of the other partners in the IEA annex 17.

The samples will be studied for hydrogen uptake and release under hydrogen flow with or without impurities added. The temperature and pressure can be varied over large ranges. The weight change of the sample is monitored as a function of time in special microbalance (TEOM, Tapered Element Oscillating Microbalance) commonly used to measure catalytic activities. The samples can also be submitted to microscopy, structure analysis (XRD) and elemental microanalysis (SEM/EDS).

Molecular modelling will be included in the work. The method has proven to be very useful for catalytic characterisation, particularly in surface catalysis of gas reactions, which is expected to be important for hydrogen storage materials.

The progress of the work will largely depend on the availability of samples. All the experimental and modelling facilities are present in-house and ready for use. A learning period is expected since this a new field to us, but production of results should be possible relatively fast. A milestone table is not enclosed now. A more scheduled plan is expected to be ready after the IEA annex 17 partner meeting in USA this summer. Until then, we will work with the samples already available.

IEA Task 17 (9 April 2001)

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IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. HC-5

Title: H-storage in nanostructured carbon and metals

Project Leader: A. Ziittel (University of Fribourg) - Switzerland Type of Project: Experimental International Collaborations: Not specified Level of Effort (Duration): 1.0 py/y (3 years)

Background

The “classical” or metallic metal hydrides used today absorb approximately 1 H/M, 1.5 mass% and 120 kg H2 m'3.of hydrogen gas at ambient temperature and pressure. The volumetric hydrogen storage density of the hydride materials is very high; however, the gravimetric density is still much lower as compared to fossil energy carriers. The main reason for the low gravimetric density is due to high atomic mass of the metallic elements. Therefore, only the sp-eiements with M < 40 g mol' offer gravimetric hydrogen capacities greater than 2.5 mass% for H/M = 1 and greater than 5 mass% for H/M = 2.

High specific surface area bulk carbon materials absorb (physisorption) reasonable amounts of hydrogen (3.5 mass%) at low temperature (77 K). On the other hand, carbon atoms chemisorbs up to 4 H/C in methane (25 mass%). However, the covalently bond hydrogen desorbes at rather high temperatures (> 500 K). Nanostructured carbon is an intermediate material between the bulk graphite (sp2) and the single isolated carbon atom (sp3). The electronic structure of the nanostructured carbon is expected to offer more stable hydrogen absorption than bulk graphite but less stable than a covalent bond. Therefore we will investigate various nanostructured carbon materials, e.g. single- and multi-walled nanotubes, high surface area graphite, and other “molecular” carbon materials. The comparison of the properties of the various materials should lead to a better understanding of the hydrogen interaction with the carbon clusters on the micro- and macroscopic scale.Several lightweight metals build compounds containing large amounts of hydrogen. These compounds are mainly ionic and rather difficult to synthesize. It was shown in the literature and confirmed in task 12, that the desorption temperature of NaAlH4 can be lowered by adding small amounts of transition metals or their oxides. The mechanism of the hydrogen desorption reaction is not yet known and the reversibility is still not satisfactory. However, this example demonstrates the possibility for the destabilization of lightweight hydrides. We will investigate the properties, desorption temperature, pressure, and reversibility of several lightweight hydrides.

Project Plans

The following methods will be applied:Structure investigation (in- and ex-situ) by means of x-ray and neutron diffraction. Hydrogen sorption measurements by means of pcT-Isothermes, Thermal desorption spectroscopy, Thermogravimetry. Surface investigation by means of photoelectron spectroscopy.

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IEA Task 17 (9 April 2001)

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Project No. HC-5 (concluded)

The following table shows the starting compounds for the planned investigation:

Material Formula M

[g mol"1]

D

[g cm"1]

Mp

[°C]

Decomp

[°C]

X

[mass%]

Lithiumboro-hydride LiBH4 21.784 0.66 268 380(75) 18.4Sodiumboro-hydride NaBH4 37.83 1.074 - 400 10.6

Potassiumboro-hydride kbh4 53.94 1.178 500 7.4Lithiumaluminum-hydride LiAlH4 37.95 0.917 125 9.5Sodiumaluminum-hydride NaAlH4 54.0 180 7.4Sodiumaluminum-hydride Na3AlH6 102.0 5.9Sodiumlithiumaluminum-hydride Na2LiAlH6 85.9 7.0Magncsiumnickcl-hydride Mg2NiH4 111.3 3.6Magnesiumiron-hydride Mg2FeH6 110.5 5.4Magncsiummangancse-hydridc Mg3MnH7 134.9 5.2

Tasks

1) Hydrogen - Carbon interaction2) Thermal desorption of the light weight hydrides3) Modification of light weight hydrides (chemical and physical)4) Investigation of the structure and the thermodynamic properties5) Hydrogen absorption of light weight metals6) Mechanism of hydrogen sorption in mainly ionic compounds

Milestones

Dates not available.

IEA Task 17 (9 April 2001)

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IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. HC-6

Title: FUCHSIA: Fuel cell and hydrogen store for integration into automobiles

Project Leader: J.D. Speight (University of Birmingham) - UK Type of Project: R&DInternational Collaborations: Johson-Matthey, Univ of Reading, Univ of Birmingham (Metallurgy and Materials, Chemistry)-UK, IFW Dresden - Germany, Univ of Fribourg - Switzerland Level of Effort (Duration): 1.0 py/y (3 years)

Background

This effort is part of the EEC ENERGIE Programme 5th Framework.

Project Plans

To investigate novel materials giving hydrogen storage of greater than 7w/o. The resulting material will be incorporated into a hydrogen store suitable for a fuel cell powered light vehicle with a range of 500km. A successful store would lead to a zero emission vehicle powered by a totally renewable energy source.

Milestones

Unavailable.

IEA Task 17 (9 April 2001)

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IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. HC-7

Title: Development and characterization of advanced materials for hydrogen storage

Project Leader: M.A. Imam, (NAVAL RESEARCH LABORATORY) - USA Type of Project: Simulation, Modeling and Experimental International Collaborations: S. Iijima (Meijo University) - Japan Level of Effort (Duration): 0.5 py/y (3 years)Background

Hydrogen is environmentally clean, a plentiful, nonhazardous, and efficient fuel. However, its storage and transportation difficulties have so far limited the use of the fuel for technological, and military purposes. One potentially practical and useful technique for hydrogen storage, is using metal, or intermetallic hydrides. To make such a system competitive the storage efficiency must be optimized by selecting a suitable system and by understanding the fundamentals of hydrogen intake in that system. A related problem is the degradation in some systems brought in by hydrogen intake. With the advent of new processing facilities, and characterization and simulation procedures, these issues can now be addressed at a very fundamental level.Project Plans

The main objectives of this research program will be achieved through a multidisciplinary approach consisting of synthesis and processing that will be integrated to characterization and analysis. Both synthesis and analysis will be complimented and reinforced by computer simulation and modeling. Synthesis and processing will involve the use of novel techniques for the production of nanostmctural metal-based samples with high hydrogen storage potential. The synthesized samples will be subsequently examined by advanced electron-optical techniques that will include the following X-ray, electron and neutron diffraction, scanning and high resolution transmission electron microscopes, (HRTEM and STEMP), electron energy loss spectroscopy (EELS), and thermogravimetric analysis (TGA). The simulation and modeling efforts will be based on crystal structure models, band structure and density of states calculations. Suitable metallic samples will be also produced by more conventional methods such as arc and induction melting. The plan is to first produce hydride forming metal samples based on the predictions of the computer simulation and modeling. Afterwards, the synthesized specimens will be characterized and studied for their hydrogen storage characteristics, efficiency of storage and stability. Following this phase, the most promising metallic-based systems will be further evaluated and their hydrogen storage properties optimized. Explore potentially high-payoff unconventional materials also using carbon nanotubes, and zirconium-based quasicrystalline materials.Milestones

Milestone Month/YearSimulation and modeling based on crystal structure 05/01Identify potential hydride materials 09/01Synthesize & characterize(phase 1 )the potential hydride materials 10/01

Based on simulation and modeling synthesize and characterize the second phase of potential hydride materials

05/02

Look into carbon nanotubes, and zirconium-based quasicrystalline alloys as potential hydrogen storage materials

05/03

Based on the outcome of phase I and phase 2, look for phase 3 12/03Final report 05/04

IEA Task 17 (9 April 2001)

IEA Hydrogen Implementing AgreementAnnex 17 - Solid and Liquid State Hydrogen Storage Materials

Project Plan

Project No. HC-8

Title: Engineering Properties of New Storage Materials

Project Leader: G. Thomas (Consultant to Sandia National Laboratories) - USA Type of Project: Modeling/ExperimentalInternational Collaboration: Will be defined as new materials are developed.Level of Effort (Duration): 0.25 py/y (3 years)

Background

The complex hydrides NaAlH4 and Na3AlH6 have demonstrated rapid and reversible hydrogen storage when doped with Ti and other catalysts. Similarly, much progress has been made in the development of carbon-based hydrogen storage materials, particularly single wall nanotubes (SWNT). However, little is known concerning the engineering of storage beds using these new materials. This proposed project will investigate the material properties required to successfully implement the use of complex hydrides and carbon nanotubes in storage devices and, using these parameters, to model the performance of such devices.

Project Plan

The project is divided into two areas: (1) determination of material properties, for example, hydrogen kinetic behavior, thermodynamic properties, thermal conductivity, heat capacity, packing density, expansion/contraction, etc., and (2) parametric modeling of bed designs to predict performance. Preferably, material property data will be available from the literature or from the investigators: however, a limited amount of experimental Work, such as thermal conductivity measurements, can be performed using Sandia facilities, when required. Modeling approaches will depend on the material and bed configuration. Both analytic and two-dimensional finite element analyses may be used.

Milestones:

1st year: Analysis of the NaAl system completed.Initial estimates of SWNT performance completed.

2nd year: Parametric analysis of complex hydrides and carbon materials completed.3rd year: Analysis of new materials developed in this timeframe.

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1-2) http://www.fe.doe.gov/coal_power/vision2l/vision2 l_sum.html

1-3) http://www.fe.doe.gov/techline/tl_fc4.html

1-4) http ://www.fe.doe.gov/techline/tl_vis21 sel 1 .html

1-5) http://www.planetark.org/dailynewsstory.cfrn7newskN8107

1-6) http://www. .drivingthefuture.org

1-7) http://aftermarket.theautochannel.eom/news/2000/05/18/958673110.l.htmli-8) (2000^3^)

1-9) PEC-1999-R-01 ^12^3^)

1-10) Euro-Quebec Hydro-Hydrogen Pilot Project (EQHHPP) PhaseII#"o# (1991)

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2- 1) http://www.gnet.org/news/newsdetail.cfm?NewsID=11217

2-2) Ballard Power Systems Inc. PROSPECTUS http ://www.ballard.com/

2-3) Ballard Power Systems Inc. Annual Report 1999 http ://www.ballard.com/annual_rep orts .asp

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2-5) http://dailynews.yahoo.eom/h/ap/20000522/bs/gm_giner_l.html

2-6) http ://www.internationalfuelcells.com/

2-7) 2000^9/1190, □ > H X AP

2-8) http://www.plugpower.com/

2-9) 1999^6/123 8, v?a—XT, PR~^-y V 4 ir—

2-10) http://gaea.calstart.org/newsSearch/selDis.html?cmd=98083193

2-11) 1999^11/112 8, 9 —

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2-13) 1999^7^ 8 8 , h n y b x GNET; http://www.gnet.org/newsdetail.cfm?NewsID=7787

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2-20) 1999^12/3160, 7 7> h»N, 'fUZ-T/H, PR”a-X7-f

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3-2) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98082540 http://www.ballard.com/viewpressrelease.asp?sPrID=90

3-3) 2OOO¥l/390, h,

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3-4) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083003

3-5) http://www.hydrogen.org/h2muc/introe.html

3-6) 2000^1/3 26 0, PR~^-X777-

3-7) 1999^9^290, 777 0 7, PR^a-^7^t-

3-8) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083374

3-9) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083221

3-10) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083196

3-11) http://unisci.com/stories/20002/0406006.htm

3-12) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083044

3-13) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083018

3-14) http://gaea.calstart.org/newsSearch/findToday.html

3-15) http://www.planetark.org/dailynewsstory.cfm7newskN5810

3-16) http://www.theautochannel.com/news/press/date/20000502/press014548.html

3- 17) Nikkei BP Network/BizTech News 11/9/2000

4- 1) http://www.ercc.com/

4-2) http://www.fe.doe.gov/techline/tl_fcelyear.html

4-3) http://biz.yahoo.com/bw/000530/ct_fuelcel.html

4-4) 1999^12/380,

4-5) http://www.theautochannel.com/news/press/date/20000620/press018658.html

4-6) http://www.fe.doe.gov/techline/tl_fc_solidox_fat.html

4-7) http://www.gnet.org/newsdetail.cfin7NewsnN9716&image 1=2 http ://www.p ubaf.b nl. gov/p r/bnlp rO33100. html

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5- 1) http://www.motorola.com/ies/ESG/3spotlight.html2000¥L^ 19 0, —

5-2) http://gaea.calstart.org/newsSearch/selDis.html?cmd=98083033

5-3) http://www.ens.lycos.com/ens/may2000/2000L-05-01-01.html

5- 4) http://www.theautochannel.com/news/press/date/20000615/press018294.html

6- 1) 1999^841170, PR-^.—* V4

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6-3) 2000^14124 0, PR-zz—

6-4) 1999^841 16 0, —

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6-6) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98082945

6-7) 1999^541200, ^ h y, PR^z% —

6-8) http://home.doe.gov/news/releases99/julpr/pr99194.htm

6-9) 1999^841 16 0, PR—

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6-12) http://gaea.calstart.org/newsSearch/selDis.html?cmd=98082969

6-13) http://www.theautochannel.com/news/press/date/20000719Zpress020939.html

6-14) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083351

6-15) 1999#12v0220, hn> h, —

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7-2) http://www.theautochannel.com/news/press/date/20000912/press025334.html

7-3) http://gaea.calstart.org/newsSearch/selDis.html7cimN98082939

7-4) http://gaea.calstart.org/newsSearch/selDis.html7cnKN98083309

7- 5) http://www.powerball.net

8- 1) http://www.fetc.doe.gov/products/power/fuelcells/overview.html

8-2) Chem. & Eng. News, 77(33),3(August 16, 1999)

8-3) E. Perry Murray , T. Tsai & S. A. Barnett, Nature, 400, 649 (12 August, 1999)8- 4) Seungdoo Park, John M. Vohs & Raymond J. Gorte, Nature, 404, 265 (16 March,

2000)9- D hj-, ssesi-^, so (2000^1/§)9-2) http://www.nfcrc.uci.edu/fcinfo/manufacturers2.htm

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■y-rx^vKM Science Institute. University of Iceland

Address : Dunhaga 3, IS—107 Reykjavik Phone # +354-525-4800 Fax # +354-552-8911

Studies on how Iceland could be gradually transformed into hydrogen economy until 2030-2040; Phasel :PEM-FC bus demo, Phase2:Reykjavik city bus fleet, Phase3:Methano! fueled PEM-FC passenger cars, Phase4:PEM-FC vessel demo, Phase5;PEM-FC fishing fleet

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M Air Products & Chemicals. Inc.

Address : 7201 Hamilton Blvd., Allentown, PA 18195-1501 Phone # +1-610-481“8336 Fax # +1-610-481-6670

H2 fuel station for 3 FC buses - Chicago Transit Authority; California FC Partnership - H2 fuel station for 50 cars at Sacramento, CA; Nevada Project - Onsite production of H2, 50 kW FC power plant, H2 & H2/natural gas fuel station for up to 27 vehicles

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H California Fuel Cell Partnership

Demonstrating more than 50 fuel cell cars and busses during 2000-2003. Partnership includes 6 auto manufacturers, 2 fuel cell companies, 3 oil companies, 5 government agencies and 6 associate partners(2 transit agencies and 4 fueling infrastructure firms)

4*±(2000*E8£)o BB jt ri<#BLTlA5o Id Clean Energy Research Institute, University of Miami

Address : Cara I Gables, FL 33124 Phone# +1-305-284-4666

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Fax # +1-305-284-4792

Hydrogen fuel, Global warming, Solar cooling & heating, hybrid solar collectors, Remote sensing, Environmental damage caused by fossil fuels

mmm^ Florida Solar Energy Center. Hydrogen Research and Applications Center

Address : 1679 Clearlake Road, Cocoa, FL Phone # +1-321-638-1001 Fax #+1-321-638-1010

Photovoltaic systems, Solar thermal systems, Energy-efficient buildings, Simulation model development, Air quality, Hydrogen from renewable resources, Pollutant detoxification, Photoelectrochemical processes, Alternative-fueled vehicle

M Florida Solar Energy Center. The University of Central Florida

Address : 1679 Clearlake Road, Cocoa, FL 32922 Phone# +1-321-638-1000 Fax#+1-321-638-1010

Photovoltaic systems, Solar thermal systems, Energy-efficient buildings, Simulation model development, Air quality, Hydrogen from renewable resources, Pollutant detoxification, Photoelectrochemical processes, Alternative-fueled vehicles

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M Gardner Cryogenics

Address : 2136 City Line Road, Bethlehem, PA 18017 Phone # +1-610-266-3734/+1-610-266-3749 Fax# +1-610-266-3752

Design and manufacture of liquid hydrogen tanks, Capacity:7kL~66kL for transportation, 6kL~230kL for storage, No loss storage of LH2 with a gas consumption rate as low as 11 m3/day is available.

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M Hvdroeen Components. Inc.

Address : 1240 North Dumont Way, Littleton, CO 80125 Phone # +1-303-791-7972 Fax#+1-303-791-7975

Metal hydride H2 storage container "SOLID-H", Hydrogen systems for fuel stations, internal combustion engines, etc., Blending equipment for H2/Natural gas mixture "HYTHANE"

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M International Association for hydrogen Energy

Address : P.O.Box 248266, Coral Gables, FL 33124 Phone # +1-305-284-4666 Fax#+1-305-284-4792

Publishes an official scientific journal "International Journal of Hydrogen Energy", organizes biennial "World Hydrogen Energy Conference"

ffi&irInternational Journal of Hydrogen Energy"Hildas l8"World Hydrogen Energy Conference"(DHfHE

M International Energy Agency. Hydrogen Program

Address : National Renewable Energy Laboratory 3311, 1617 Cole Blvd., Golden, CO

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7kstmnMuxh 3/7 V-y

Phone # +1~303—384—6355 Fax# +1-303-384-6103

IEA was founded in 1974, as an agency in OECD. Hydrogen Program consists of international collaborations for hydrogen energy systems including research tests, Task12:H2 storage in MH & carbon, Taskl 3:Design & optimization of intenerated systems, etc.

•T _t _ -fc n.Jk -Hr J.-l- A. % — — i ^ —n - i i ebi / i . 11 # JL<___ I . -=fcr 4fc.il sM. «I / i_L_ iLi— 11.-1. 4fcll 'X

Lawrence Livermore National Laboratory

Address : University of California, Livermore, CA 94551

Hydrogen fuel, Solid Oxide FC, Zinc/Air FC, Cryotank storage of hydrogen and natural gas, High-temperature steam elecrtolyzer for hydrogen production, Carbon dioxide sequestration, Advanced flywheel, Fission energy

M Los Alamos National Laboratory

Address : MS K 765, Los Alamos, NM 87545 Phone # +1-505-665-9336 Fax # +1-505-665-2992

Fuel cell Technologies, Carbon sequestration, Zero-emission coal-fueled power plant (DOE Vision 21 program), Green chemistry

7 AX ^U->^5XhU-M National Hydrogen Association

Address : 1800 M Street, NW Suite 300N Washington, DC 20036-5802 Phone # +1-202-223-5547 Fax # +1-202-223-5537

Nonprofit membership organization with members from industries, universities, etc. Its mission is to foster development of hydrogen technologies and their industrial/commercial applications, and to promote hydrogen energy systems.

MlblcSAU g MtLXl'&oMSchatz Energy Research Center. Humboldt State University

Address : Areata, CA 95521-8299 Phone # +1-707-826-4345 Fax# +1-707-826-4347

Solar hydrogen/fuel cell plant with 192 solar panels, 6kW electrolyzer (1990), PEM fuel cells for portable generator and vehicles

98 SRI international

Address : 333 Ravenswood Avenue, Menlo Park, CA 94025 Phone # +81-3-5251-1764 Fax# +81-3-5251-1774

Hydrogen safety, Solid oxide fuel cells, High-temperature polymer electrolytes for hydrogen production

88 University of Florida, Department of Mechanical Engineering

Address : 228 MEB, P.O.Box 116300, Gainesville, FL Phone #+1-352-392-7821

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Fax# +1-352-392-1071

Hydrogen liquefaction systems and processes, Hydrogen storage (liquid) systems

7kS$lkvX7.AM70nizX> ;M7KSItSvXtAUniversity of Hawaii. Department of Chemistry

Address : 2545 McCarthy Mall, Honolulu, HI 96822 Phone#+1-808-956-2769 Fax# +1-808-956-5908

Catalytically enhanced complex aluminum hydrides as hydrogen storage materials for vehicular applications

M King’s College London, Division of Life Science

Address : 150 Stanford St, Waterloo, London SE1 SWA Phone # +44-20-7848-4317 Fax# +44-20-7848-4500

H2 production with cyanobacteria in outdoor bioreactors, Sustained H2 production from Anabaena Variabilis mutant strain PK84 in helical photobioreactors set up outdoors using natural sunlight as energy source, Nitorgenase & hygrogenase

mmms wj7^-<tr>7// <>ru yie jtSTkSMm. mmciemuznim#C:%5iJ&#4](7)Anabaena VariabilisWH:$PK84$-fflL Vz 6 —;JS<h"7&

M Ballard Power Systems

Address : 9000 Glenlyon Parkway, Burnaby BC V5J 5J9 Phone # +1-604-412-3195 Fax# +1-604-412-3100

PEM fuel cells, PEM fuel cell systems; Alliances with DaimlerChrysler & Ford for automotive applications, GPU International Inc., ALSTOM France & Ebara Corp. for stationary power generators, Coleman Powermate for portable & low power stationary applict’ns

A5—<7^<X5—SltiSffl), GPU International. ALSTOM France^)Coleman Powermate#i&ttjti

3HCANMET Energy Technology Center

Address : 580 Booth Street, Ottawa K1A 0E4 Phone # +1-613-996-8201 Fax # +1-613-995-9584

CANMET is a R&D arm of NRCan, Natural Resources Canada. H2 Production(electrolysis), UtilizationCsmall integrated system, personal fuel appliance), Storage(MH, C-nanotubes, magnetic refrigerants), Safety, Fuel cells(new PEMs, reversible PEM, SOFC stack)

CANMETtiNRCan(*d-yS;Ji^i)(DR&DTMS'e/3d-y(D7kS/FC^Py^A$mm. 7kSM(7k®M)>7kSlyE(MH% BSvtSX 7kSCD$^t4x ##mm(#mPEM.oimj^J^mPEM, SOFCX^V^)

SS Hydro-Quebec Institute of Research

Address : IREQ, 1800 Blvd. Lionel Boulet, Varennes, Quebec J3X 1S1 Phone # +1-450-652-8234 Fax# +1-450-652-8424

Elecrtocatalysis, Fuel cells, Electrolyzer, Properties of materials in relation to H2, Theoretical and quantum mechanical aspects of metal-hydrogen interactions,

—144—http://www.enaa.or.jp/WE-NET/kenkyu/countryj.html 01/04/23

7kstmiiEuxh 5/7 v-y

Hydrogen economy, Greenhouse gases and environment

TkSSiiS, ;Sa«1b*’7.iiS»F=1liHU Instittut de Recherche sur 1’Hvdrogene. Universite du Quebec a Trois-Rivieres

Address : C.P. 500, Trois-Rivieres, Quebec G9A 5H7 Phone # +1-819-376-5139 Fax # +1-819-376-5164

H2 storage(adsorption, magnetic liquefaction, metal hydrides), TransportCdefect detection in tanks, contaminants detection in a gas, thermodynamics),Safety(hazardous assessment, hydrogen flame propagation, source book), UsesOC engine, renewable energy)

7k#%me#), fix

Institut de recherche d’Hydro-Quebec, Technologies Emergentes de Production et de Stockage

Address :1790 Boulevard Lionel-Boulet, Varennes, Quebec J3X 1S1 Phone # +1-450-652-8134 Fax # +1-450-652-8334

Nanocrystalline metal hydrides, such as Mg based alloys, complex hydrides, AB5 type, AB type and chemical hydrides; Metal hydride storage containers

7k#%m^#(7^vOAe#. 3>^Uv<7X7k#ib#. AB5SL AB§k 7k#ik

B Laboratorire d'Electrochimie et de Materiaux Energetioues

Address : Ecole Polytechnique de Montreal, C.P. 6079, Centre-ville, Montreal, Qc, H3C 3A7Phone # +1-515-340-4725 Fax # +1-514-340-4468

Polymer electrolyte membrane fuel cells, Water electrolysis, Electrocatalysis, Membranes, Bipolar plates, Cell design

pEM§m#m;K wm&l mmm

■S8BM Korea Advanced Institute of Science and Technology. Advanced Functional

Materials Laboratory

Address : 373-1 Kuseong-Dong, Yuseong-ku, Taejeon 305-701 Phone # +82-42-869-3353 Fax # +82-42-869-8910

Ni-H battery (AB2, AB5, V-based alloy, Mg-based alloy), Metal hydride heat pump, Carbon nanotube for hydrogen storage, Thin film

-^/;i-7kSl:;th(AB2§y££% ab5M££>MHt-h7k°>^ mmm

Energy Research Institute. King Abdulaziz City for Science and Technology (KACST)

Address : P.O.Box 6086, Riyadh 11442 Phone # +966-1-4813514 Fax # +966-1-4813880

Solar hydrogen production, Fuel cell (PAFC/PEM)

*l!*;7kSEi£s PAFC/PEM)

Linde Krvotechnik AG

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7kS9f%OTUXH 6/7 v-y

Address Daettlikonerstrasse 5, P.O.Box CH-8422, Pfungen Phone # +41-52~304-0518 Fax # +41-52-304-0550

Hydrogen liquefaction plant in capacity of 5 - 250 g/s (design, installation, commissioning, operation)

ASfclfcIStiiOKth mm. 5-250g/s)

Institute National der Tecnica Aerosoaciai (INTA)

Address : Ctra San Juan-Matalascanas Km33, 21130 Mazagon, Huelva Phone # +34-959-208849 Fax # +34-959-208828

Solar hydrogen production, Integration of PEM fuel cell in power plants, Characterization and testing of components

■ K-f'VHCONSULECTRA Unternehmensberatung GmbH

Address : Weidestrasse 126, D-22083 Hamburg Phone # +49-40-278 99-243 Fax #+49-40-278 99-211

A subsidiary of HEW (Hamburgische Electricitaets-Werke AG), consulting and assisting hydrogen project such as EIHP(European Integrated Hydrogen Project), WEIT (Wasserstoff Energie Transport Integration), ARGE MUC(a demo project in Hamburg of CGH2 station)

HEW(/#%) 7kSXni/x<7H7)zi>th;U-r>f>^[ EIHP(European Integrated Hydrogen Project), WEIT(Wasserstoff Energie Transport Integration), ARGE MUC(a demo project in Hamburg of CGH2 station)#]

MForschuneszentrum Juelich GmbH (Institute for Materials and Process in EnergySystems, etc.)

Address : D-52425 JuelichPhone # +49-2461-61-4744/+49-2461-61-3525Fax # +49-2461-61-2840/+49-2461-61-6695

One of the 16 Helmholtz Research centers, Energy (nuclear fusion, fuel cells), Environment (atmospheric chemistry, radioagronomy, environmental specimen bank); Autonomous house system, PEFC power train (©Institute for Materials & Processes in Energy Sys)

l6(7)^;izA7h;iz'7E^FJr(D1o0 flMBMtSISA'K 3ft»Mmetmaxk#. K#4fflfr(0-l5OC);

M Forum fuer Zukunftsenergien e.V. EFO Energie GmbH

Address : Godensberges Allee 90, 53175 Bonn Phone # +49-228-95956-0 Fax # +49-228-95956-50

Organizing HYFORUM2000, The international hydrogen energy forum 2000, Policy-Business-Technology

/ WXf—5A2000#±@. iSH3B Fraunhofer institute for Solar Energy Systems

Address : Oltmannstrasse 5, 79100, Freiburg Phone # +49-761-4588-194 Fax # +49-761-4588-320

Thermal use of solar energy, Photovoltaics, Solar architecture, Electric power supplies, Chemical energy conversion, Rational use of energy, Grid-independent solar house

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xmmm, Aiwti, g^y-5-/\ox(77^;u^rfixPnic5$TbtL/c5lllEJir\ n^^bCD-tJ]0x^;^H^^LIcS^S8.m*&*&m£t&tzto\zpv**s2i-)\,% m»HS7k*»««. mmfc,

SEJ German Aerospace Center (DLR)

Address : Pfaffenwaldring 38-40, D-70569, Stuttgart Phone # +49-711-6862-481/+49-711-6862-481 Fax # +49-711-6862-747

SOFC R&D Planar thin-film cells, Vacuum plasma spray techniques, Protective coatings for metallic bipolar plates, In situ synthesis of perovskite powder and layer by RF plasma process, Cell and stack design and modeling, System analysis

RF^5X77°otxlcj:6^ax±i<F0m#,littfx vXiFAM(=iXk m*§ti)

MStadwerke Muenchen GmbH. Pep. Unternehmenssteuerune

Address : Blumenstrasse 19, D-80287, Muenchen Phone #+49-89-2361-5085 Fax # +49-89-2361-4452

Studies on the mixture of H2 into the gas networO 994), Small stationary FC co-generation plantsO 997), FC co-generation plant on the electric distribution net (2000), "Public Demonstration of PEM FC as miniature household co-generation plants in Munich"

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SI Wasserstof-Gesellschaft Hamburg e.V.

Address : Trostbruecke 1, D-20457 Hamburg Phone # +49-40-36808-249 Fax # +49-40-36808-200

A non-profit organization of scientific-technical character. Aim is to explore and enforce the introduction of the hydrogen technology into existing energy systems. Promotes hydrogen projects predominantly in the field of road transport

f4^Milc^r>E>#^J^I3l^-C:\S^0x^;u^-vX-TA/N07kSM0SA

M Institute for Energiteknikk (Institute for Energy Technology)

Address : P.O. Box 40, N-2027 Kjeller Phone # +47-63 80 60 00 Fax # +47-63 81 29 05

Hydrogen storage in metal hydride and carbon materials, Analysis of H2-systems, hydrogen production from fossil fuel, Laboratory testing and regulation of components in autonomous systems

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